High-flux mold for spark plasma sintering and sintering equipment thereof

Abstract

The utility model provides a high-flux mold for spark plasma sintering and sintering equipment thereof, and relates to the technical field of sintering, the high-flux mold comprises at least one pressure head and a porous mold; the multi-hole die comprises one or two hole opening faces, and a plurality of closed holes are formed in the hole opening faces. The closed holes are formed in the vertical direction of the porous mold, the hole diameters of the multiple closed holes are the same, and the closed holes are used for containing sintering raw materials; a plurality of sub-pressure heads are arranged on the pressure head, and the sub-pressure heads are in one-to-one correspondence with the plurality of closed holes; and the pressure head comprises a large pressure head. By adopting the high-throughput mold provided by the embodiment of the utility model, samples can be prepared on a large scale through one-time spark plasma sintering, so that the efficiency and sustainability of a spark plasma sintering process are improved, and the component screening and optimization of the samples are further accelerated.

Description

Technical Field

[0001] The utility model relates to the technical field of sintering, and particularly relates to a high-throughput mold for spark plasma sintering and a sintering device thereof. Background Art

[0002] The research on preparing new materials by spark plasma sintering (SPS) at home and abroad mainly focuses on: ceramics, cermets, intermetallic compounds, composite materials and functional materials, etc. Among them, the most studied are functional materials, including thermoelectric materials, magnetic materials, functionally graded materials, composite functional materials and nano-functional materials, etc. SPS is a relatively mature powder sintering technology. It can sinter samples during the pressurization process and introduce pulsed current into the sintering process. When pulsed current is introduced into the electrodes, discharge plasma is generated instantaneously, enabling each particle inside the sintering raw materials to uniformly generate its own Joule heat and activate the particle surface. In addition, the plasma generated by the pulsed current and the pressurization during the sintering process are beneficial to reducing the sintering temperature of the powder, so that the powder can be quickly sintered and densified. This technology has the characteristics of low voltage and high current.

[0003] In the prior art, the vast majority of SPS devices are designed for large-size samples and large-scale industrial production. The sample preparation process is time-consuming and energy-consuming, and only one sample can be prepared at a time, and it is impossible to realize the synthesis and sintering of a large number of samples at one time. Although some prior technologies can prepare multiple samples at one time, for multiple samples, the sintering and pressurization at one time cannot conduct electricity uniformly, so the uniformity of the samples cannot be guaranteed, which may lead to the failure of sample sintering.

[0004] Therefore, in the technical field of sintering, only one uniform sample can be prepared by one-time spark plasma sintering treatment, and its low preparation efficiency and high preparation cost have become technical problems to be solved urgently at present. Summary of the Utility Model

[0005] To solve the above problems, the utility model provides a high-throughput mold for spark plasma sintering. The high-throughput mold includes at least one pressure head and a porous mold;

[0006] The porous mold includes one or two open surfaces, and a plurality of closed holes are formed on the open surface; the closed holes are formed along the vertical direction of the porous mold, and the apertures of the plurality of closed holes are the same. The closed holes are used for placing sintering raw materials;

[0007] A plurality of sub-pressure heads are arranged on the pressure head, and the sub-pressure heads correspond to the plurality of closed holes one by one; the pressure head includes a large pressure head.

[0008] Further, the closed holes formed on one of the two perforated surfaces are arranged in a staggered manner with respect to the closed holes formed on the other perforated surface.

[0009] Further, the closed holes formed on one of the two perforated surfaces are arranged in alignment with the closed holes formed on the other perforated surface.

[0010] Further, the closed holes formed on the perforated surface are evenly distributed.

[0011] Further, the arrangement distribution of the closed holes is orthogonal.

[0012] Further, the arrangement distribution of the closed holes is close-packed.

[0013] Further, the high-throughput mold includes a spacer block, and the spacer block covers the sintering raw material and is located on the side close to the sub-punch.

[0014] Further, the high-throughput mold includes graphite paper, and the graphite paper is arranged at the bottommost part of the closed holes.

[0015] Further, the lengths of the plurality of sub-punches are the same.

[0016] In a second aspect, the present invention provides a spark plasma sintering device, and the spark plasma sintering device includes the high-throughput mold described in the first aspect above.

[0017] Compared with the prior art, the present invention has the following advantages:

[0018] The present invention provides a high-throughput mold for spark plasma sintering and its sintering device, which relates to the technical field of sintering. The high-throughput mold includes at least one punch and a porous mold; the porous mold includes one or two perforated surfaces, and a plurality of closed holes are formed on the perforated surfaces; the closed holes are formed along the vertical direction of the porous mold, and the apertures of the plurality of closed holes are the same, and the closed holes are used for placing sintering raw materials; a plurality of sub-punches are arranged on the punch, and the sub-punches and the plurality of closed holes are in one-to-one correspondence; the punch includes a large punch. By using the high-throughput mold provided by the embodiment of the present invention, a large number of samples can be prepared by one-time spark plasma sintering, thereby improving the efficiency and sustainability of the spark plasma sintering process, and further accelerating the component screening and optimization of the samples. Description of the Drawings

[0019] To more clearly illustrate the technical solution of the present utility model, the following will briefly introduce with reference to the accompanying drawings. Obviously, the accompanying drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0020] Figure 1 Schematic diagram of a high-throughput mold for spark plasma sintering provided by an embodiment of the present utility model;

[0021] Figure 2 Schematic diagram of a second high-throughput mold for spark plasma sintering provided by an embodiment of the present utility model;

[0022] Figure 3 Cross-sectional view of a high-throughput mold for spark plasma sintering provided by an embodiment of the present utility model;

[0023] Figure 4(a) is a cross-sectional view of a second high-throughput mold for spark plasma sintering provided by an embodiment of the present utility model;

[0024] Figure 4(b) is a cross-sectional view of a third high-throughput mold for spark plasma sintering provided by an embodiment of the present utility model;

[0025] Figure 5 (a) is an arrangement mode of closed pores in the high-throughput mold provided by an embodiment of the present utility model;

[0026] Figure 5 (b) is another arrangement mode of closed pores in the high-throughput mold provided by an embodiment of the present utility model;

[0027] Figure 6 Schematic diagram of a sintering device for spark plasma sintering provided by an embodiment of the present utility model. Detailed implementation manners

[0028] The following details the embodiments of the present utility model. The examples of the embodiments are shown in the accompanying drawings, where the same or similar reference numerals represent the same or similar elements or elements with the same or similar functions from beginning to end. The embodiments described below by referring to the accompanying drawings are exemplary and are only used to explain the present utility model, and should not be construed as a limitation to the present utility model.

[0029] In the description of the present utility model, it should be understood that for the orientation description, such as up, down, front, back, left, right, etc., the orientation or positional relationship indicated is based on the orientation or positional relationship shown in the accompanying drawings. It is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation to the present utility model.

[0030] In the description of the present utility model, "several" means one or more, "more" means more than two, "greater than", "less than", "exceed" etc. are understood to exclude the number itself, and "above", "below", "within" etc. are understood to include the number itself. If there is a description of "first" or "second", it is only used for the purpose of distinguishing the technical features, and cannot be understood as indicating or implying the relative importance or implicitly indicating the number of the indicated technical features or implicitly indicating the order of the indicated technical features.

[0031] In the description of the present invention, unless otherwise clearly defined, terms such as setting, installing, connecting, etc. should be understood in a broad sense, and technicians in the relevant technical field can reasonably determine the specific meanings of the above terms in the present invention based on the specific content of the technical solution.

[0032] In addition, the technical solutions between the various embodiments of the present invention can be combined with each other, but it must be based on the fact that ordinary technicians in the field can implement it. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0033] Thermal barrier coating materials, such as 6-8% Y 2 O 3 Stable ZrO 2 Ceramic material (yttria stabilized zirconia, referred to as 8YSZ) has a high melting point (2973K), fracture toughness, thermal expansion coefficient (11.5×10 -6 K -1 ) and low thermal conductivity (1273K, 2.12W / (m·K)), is currently the most widely used thermal barrier coating material. However, with the increasing service temperature of aircraft engines and gas turbines, the 6-8YSZ thermal barrier coating material will undergo a phase transition from tetragonal to monoclinic phase, which will be accompanied by a change in the volume of the coating. Eventually, a large number of cracks will form in the coating during the thermal cycle, leading to coating peeling and failure of the thermal barrier coating system. In addition, a main component of CaO-MgO-Al 2 O 3 -SiO 2 The silicate environmental deposits (CAMS) are also an important reason for the high-temperature corrosion failure of the ceramic layer on the blade surface.

[0034] Domestic and foreign researchers have carried out a lot of work to improve the high temperature phase stability and molten salt corrosion resistance of YSZ thermal barrier coatings through doping modification, which is mainly reflected in rare earth oxide unit doping, multi-element doping and other element doping modification. The rare earth oxides doped in the YSZ coating unit mainly include La 2 O 3 、CeO2 , Sm 2 O 3 , Sc 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , etc. The multi-doped YSZ coatings include YbGdYSZ (Yb 2 O 3 , Gd 2 O 3 , Y 2 O 3 co-stabilized ZrO 2 ), GdCeYSZ (Gd 2 O 3 , Ce 2 O 3 , Y 2 O 3 co-stabilized ZrO 2 ), ScYbYSZ (Sc 2 O 3 , Yb 2 O 3 , Y 2 O 3 co-stabilized ZrO 2 ), etc.

[0035] However, the composition optimization of the multi-doped system ZrO 2 -Y 2 O 3 -RE 2 O 3 will bring a huge workload. Optimizing the composition by the "trial and error method" is not only inefficient, but also the samples of different batches will have unpredictable factors affecting the experimental results due to differences in experimental conditions, operators, etc., and even affect the optimization results of the material system.

[0036] In order to accelerate the composition optimization and screening of the material system prepared by spark plasma sintering, the present utility model provides a high-throughput mold for spark plasma sintering, as shown in any one of Figure 1 to Figure 4. The high-throughput mold includes at least one punch 1 and a porous mold 2; the porous mold 2 includes one or two open surfaces 21, and a plurality of closed holes 22 are provided on the open surface 21; the closed holes 22 are opened along the vertical direction of the porous mold 2, and the diameters of the plurality of closed holes 22 are the same. The closed holes 22 are used to place sintering raw materials 23; a plurality of sub-punches 11 are provided on the punch 1, and the sub-punches 11 correspond to the plurality of closed holes 22 one by one; the punch includes a large punch 12.

[0037] Among them, the material of the high-throughput mold is graphite, which can endow the high-throughput mold with excellent electrical conductivity and high-temperature stability, so that its mechanical properties and structural integrity can be maintained at a relatively high sintering temperature.

[0038] By using the high-throughput mold provided by the embodiment of the present utility model, a large number of samples can be prepared in one-time spark plasma sintering, thereby improving the efficiency and sustainability of the spark plasma sintering process, and further accelerating the component screening and optimization of the samples.

[0039] Compared with the mold for ordinary spark plasma sintering, by using the high-throughput mold provided by this embodiment, different sintered samples can be synthesized in large quantities at one time under the same experimental conditions for component screening and optimization of the samples. Thus, the sample with the best performance can be quickly screened out from a batch of samples, which has the advantages of reduced variables, reduced experimental errors, and improved reliability of data results.

[0040] Among them, the same experimental conditions refer to that after one-time sintering is completed, the sintering temperature, sintering pressure, and heat preservation time of this batch of samples are the same; synthesizing different sintered samples means setting the mass ratio of each component of the sintering raw material to be different, and / or setting the powder particle size of each component to be different for component screening and optimization of the samples. Since the sintering temperature, sintering pressure, and heat preservation time of one-time sintering are the same, using the high-throughput mold provided by this embodiment can reduce variables, without the need to control the sintering temperature, sintering pressure, and heat preservation time of each sintering, thereby reducing the errors caused by multiple sinterings and improving the reliability of the results of sample component screening and optimization.

[0041] As Figure 3 shown in or Figure 4, the closed pores 22 are non-penetrating holes, and the sintering raw materials are placed in the holes.

[0042] As Figure 1 shown in any one of to Figure 4, the opening surface 21 is the surface on the side where the closed pores 22 are opened. The opened closed pores 22 are opened along the vertical direction of the porous mold 2, and this vertical direction is the direction towards the large punch 12; the large punch 12 is a horizontal large punch, and the large punch 12 is used to play a buffering and connecting role between the multiple sub-punches 11 and the upper and lower punches of the spark plasma sintering equipment to protect the upper and lower punches of the spark plasma sintering equipment from being damaged. If the sub-punch 11 directly contacts the upper and lower punches of the spark plasma sintering equipment, when a certain sub-punch 11 is not placed horizontally, stress concentration will occur at the contact between the two, and pits will be generated at the upper and lower punches at the stress concentration point, resulting in the inability of the spark plasma sintering equipment to perform the next spark plasma sintering.

[0043] As Figure 1As shown in any one of FIGS. 1 to 4, there is a matching sub-punch 11 for each closed hole 22. The large punch 12 evenly distributes pressure and pulsed current on each sub-punch 11, and each sub-punch 11 then applies pressure and pulsed current to the sintering raw material in the corresponding closed hole 22 to enable the sintering raw material to perform spark plasma sintering.

[0044] As Figure 1 or Figure 3 shown, the porous mold 2 includes an open-hole surface 21, the punch includes a large punch 12, and the closed holes 22 are opened in the direction towards the large punch 12, and there is only one opening direction. At this time, the provided high-throughput mold is a single-layer structure and can perform single-layer spark plasma sintering.

[0045] As Figure 2 or as shown in FIG. 4, the porous mold 2 includes two open-hole surfaces 21, the punch includes two large punches 12, and the closed holes 22 are opened simultaneously in the direction towards the two large punches 12, and there are two opening directions. Correspondingly, as shown in FIG. 4(a) or FIG. 4(b), non-penetrating closed holes 22 are opened on both open-hole surfaces 21. At this time, the provided high-throughput mold is a double-layer structure, and this high-throughput mold can achieve upper and lower layers, thus making full use of the space of the high-throughput mold. Compared with Figure 1 or Figure 3 the single-layer structure high-throughput mold shown, the double-layer structure high-throughput mold can double the number of spark plasma sintering samples.

[0046] As Figure 1 shown in any one of FIGS. 1 to 4, the apertures of the closed holes 22 in the high-throughput mold provided in this embodiment are the same. When performing spark plasma sintering with the high-throughput mold provided in this embodiment, the pulsed current is directly applied to the high-throughput mold. The upper punch and the lower punch of the spark plasma sintering equipment act as carriers of the current while applying pressure to the high-throughput mold. The discharge plasma generated by the current enables each particle inside the sintering raw material to uniformly generate its own Joule heat, activating and heating the particle surface. At the same time, part of the current passing through the high-throughput mold heats the high-throughput mold, enabling the high-throughput mold to transfer heat to the sintering raw material inside the mold. The temperature of the sintering raw material rises due to heat transfer, starts to shrink, generates a certain density, and increases with the increase in temperature until the shrinkage ends after reaching the sintering temperature, and the relative density reaches the maximum to complete the spark plasma sintering. Since current is used for sintering during spark plasma sintering, only when the apertures of the closed holes 22 are the same can uniform conduction be achieved, thereby ensuring the uniformity of the samples.

[0047] If the pore diameters of the closed pores are different, for example, the pore diameter of the closed pore at the center of the high-throughput mold is 39 mm, and the pore diameters of the closed pores around it gradually decrease along the edge direction of the high-throughput mold, and the pore diameter of the closed pore at the outermost edge of the high-throughput mold is 9 mm. At this time, when using this high-throughput mold for spark plasma sintering, after the current is evenly distributed on the sub-platen 11, due to the different pore diameters of the closed pores 22, the resistance differences on each closed pore 22 are extremely large, and then it is impossible to ensure that the sintering temperature and sintering pressure of the sintering raw materials in each closed pore can reach the preset temperature and pressure, thus it is impossible to ensure the uniformity of the sample.

[0048] The high-throughput mold provided by this embodiment has customizability; in the single-layer structure high-throughput mold as shown in Figure 1 or Figure 3 or the double-layer structure high-throughput mold as shown in Figure 2 or Figure 4, there are no specific restrictions on the shape of the closed pores 22, the number of the closed pores 22, and the fixed value of the pore diameter of each closed pore 22, and they can be customized according to the needs of customers.

[0049] Exemplarily, if the customer's requirement is a sintered sample in the shape of a circle, a square or a hexagon, then the shape of the closed pores 22 is set to a circle, a square or a hexagon. As shown in Figure 1 and Figure 2 , the shapes of the closed pores 22 are all circles. Exemplarily, with the rapid development of various material characterization and performance measurement technologies in recent decades, the requirements for the size of material samples are becoming more and more miniaturized and micro-ized. Therefore, when the customer needs a small-sized sample, the pore diameter of each closed pore 22 is set to any value in the range of 1 mm to 10 mm, and accordingly, the number of the closed pores 22 can be obtained according to the widths of the upper and lower platens of the spark plasma sintering equipment. Exemplarily, if the customer needs a structural part sample to optimize the mechanical properties of the sample, then the pore diameter of each closed pore 22 is set to any value in the range of 20 mm to 40 mm, and the number of the closed pores 22 is also obtained according to the widths of the upper and lower platens of the spark plasma sintering equipment. For example, if the widths of the upper and lower platens of the spark plasma sintering equipment are 100 mm and the pore diameter of the closed pore 22 is set to 20 mm, then four closed pores 22 can be set.

[0050] In this embodiment, the samples sintered in the high-throughput mold can be rare earth oxide stabilized zirconia samples, or any other types of samples with a sintering process close to that of rare earth oxide stabilized zirconia can be sintered in one furnace at a time; specifically, if the preset sintering temperature for sintering a rare earth oxide stabilized zirconia sample is 1500 °C, the preset sintering pressure is 50 MPa, and the preset holding time is 5 min; the sintering conditions for another type of sample are also a certain temperature, pressure and time, that is, the sintering process is close, then the sintering raw materials of this sample can be put into the high-throughput mold of this embodiment for spark plasma sintering.

[0051] The sintering raw material 23 filled in the high-throughput mold can be sintered and taken out of the furnace at one time, and any material that can be placed flat inside the closed hole 22; based on the pore size of the closed hole 22, the filled sintering raw material can be a block raw material, a laminated raw material, or a powder-block raw material, and finally a complete sheet material or block material can be sintered. Specifically, when the filled sintering raw material is less, a sheet material can be sintered; when the filled sintering raw material is more and the filling in the closed hole 22 is thicker, a block material can be sintered. Further, the sintering raw material filled in the high-throughput mold provided by the present utility model does not select a rod material. If too much sintering raw material is filled in the closed hole 22 and a rod material is sintered as a result, since the filled sintering raw material in the closed hole 22 is thicker, uniform conduction cannot be achieved during the spark plasma sintering process, and further the sintering temperature and sintering pressure of each sintering raw material 23 in the closed hole 22 cannot reach the preset temperature and pressure, thus the uniformity of the sample cannot be guaranteed.

[0052] The high-throughput mold provided in this embodiment can also be used for hot press sintering to improve the efficiency and sustainability of the hot press sintering process, thereby accelerating the composition screening and optimization of the sample; since no pulsed current needs to be introduced for hot press sintering, the pore diameters of the closed holes 22 in the high-throughput mold can be set to be the same or different.

[0053] In some embodiments of the present utility model, as shown in FIG. 4(a), the closed holes 22 opened on one of the two opening surfaces 21 are arranged in a staggered manner with the closed holes 22 opened on the other opening surface 21.

[0054] In some embodiments of the present utility model, as shown in FIG. 4(b), the closed holes 22 opened on one of the two opening surfaces 21 are arranged in an aligned manner with the closed holes 22 opened on the other opening surface 21.

[0055] In this embodiment, as shown in FIG. 4(a) or FIG. 4(b), it is a high-throughput mold with a double-layer structure. The closed holes 22 in the upper layer and the closed holes 22 in the lower layer of the high-throughput mold are all non-penetrating holes. The complete staggered arrangement or aligned arrangement of the closed holes 22 in the upper layer and the closed holes 22 in the lower layer can further ensure the stability of the pulsed current, thereby ensuring the uniformity of the sample.

[0056] In some embodiments of the present utility model, as Figure 1 shown in any of FIGS. 4, the closed holes 22 opened on the opening surface 21 are evenly distributed.

[0057] Among them, the position distributions of all the closed holes 22 are uniform, that is, the intervals between the closed holes 22 are the same, and the interval between the closed hole 22 and the adjacent closed hole 22 is a fixed value;

[0058] In this embodiment, by precisely controlling the positions of the closed pores 22 in the porous mold 2, the wall thickness between the closed pores 22 is uniform, so as to effectively guide and disperse the pressure and heat brought by the pulsed current during spark plasma sintering, thereby maintaining a uniform heat field across the entire high-throughput mold and avoiding pressure and heat concentration on a single sample. If the distribution of the closed pores 22 is uneven, the wall thickness between the closed pores 22 will be inconsistent. When pressure and pulsed current are applied to the high-throughput mold during sintering, the samples in the closed pores 22 with thinner walls will be subjected to greater pressure and current, while the samples in the closed pores 22 with thicker walls will be subjected to smaller pressure and current, or even no pressure and current at all, resulting in different sintering temperatures and pressures for the samples in the thinner-wall and thicker-wall regions. Therefore, if the distribution of the closed pores 22 is uneven, on the one hand, it is impossible to ensure that the sintering temperature and pressure in each closed pore 22 reach the preset temperature and pressure, thus unable to guarantee the uniformity of the samples; on the other hand, the porous mold 2 in the thinner-wall region may break due to greater pressure, leading to the failure of high-throughput mold sintering or even the inability to continue with spark plasma sintering.

[0059] In some embodiments of the present utility model, as Figure 5 (a) shows, the arrangement distribution of the closed pores 22 is orthogonal.

[0060] In this embodiment, the closed pores 22 are arranged in a quadrilateral distribution to protect the porous mold 2 from breaking during spark plasma sintering; among them, one closed pore 22 is provided at each vertex of the quadrilateral, so that a group of four closed pores 22 forms the smallest unit in this arrangement; exemplarily, as Figure 1 or Figure 2 shows, the arrangement distribution of the closed pores 22 is orthogonal.

[0061] Compared with the close-packed distribution method, the orthogonal arrangement is easier to mark the samples.

[0062] In some embodiments of the present utility model, as Figure 5 (b) shows, the arrangement distribution of the closed pores 22 is close-packed.

[0063] In this embodiment, the closed pores 22 are arranged in a regular hexagon distribution to protect the porous mold 2 from breaking during spark plasma sintering; among them, one closed pore 22 is provided at each vertex of the regular hexagon, and one more closed pore 22 is provided at the middle position, so that a group of three closed pores 22 forms the smallest unit in this arrangement.

[0064] Compared with the orthogonal distribution method, on a high-throughput mold of the same size, more closed pores 22 are opened in the close-packed arrangement, resulting in more sintered samples, and this distribution method has the advantage of large space utilization.

[0065] In some embodiments of the present utility model, asFigure 3 As shown in FIG. 4, the high-throughput mold includes a spacer block 24, which covers the sintering raw material 23 and is located on one side close to the sub-punch 11.

[0066] In this embodiment, the hole heights of the closed holes 22 are adjusted to be consistent by the spacer blocks 24, so that each sub-punch 11 vertically covers each spacer block 24, so that each sintering raw material 23 is subjected to pressure and pulsed current, and each sintering raw material 23 can effectively achieve spark plasma sintering.

[0067] Specifically, since the length of each sub-punch 11 is fixed, and the filling amounts of the sintering raw materials 23 in different closed holes 22 can be different, at this time, the spacer blocks can be used for adjustment to adjust the heights of the closed holes 22 to be consistent. In this way, each sub-punch 11 can vertically cover each spacer block 24. If one of the sub-punches 11 does not cover its corresponding spacer block 24, the sintering raw material located below the spacer block 24 cannot be sintered; if one of the sub-punches 11 covers its corresponding spacer block 24 but does not vertically cover its corresponding spacer block 24, stress concentration will occur, which will further cause damage to the upper and lower membrane punches of the spark plasma sintering equipment, resulting in sintering failure and the sintering equipment being unable to perform the next spark plasma sintering.

[0068] Exemplarily, when the target samples are two sheet-shaped ceramic materials and the preset thicknesses of the target samples are 1 mm and 10 mm, since the filling amount of the 1-mm target sample is less, the closed hole 22 corresponding to its sintering raw material 23 can be dug slightly shallower, and the closed hole 22 of the other sample can be dug deeper. After the high-throughput mold is made, the graphite paper 25 and a quantitative sintering raw material 23 are sequentially placed in the closed hole 22. At this time, the heights of the two sintering raw materials 23 after being filled do not necessarily remain on the same horizontal plane. If they are not on the same horizontal plane, two spacer blocks 24 are respectively covered on the sintering raw materials 23. The heights of the two spacer blocks are different, and after covering, the two sub-punches 11 will vertically cover the two spacer blocks 24 to ensure that the two sintering raw materials 23 can be successfully sintered. In addition, the closed hole 22 cannot be set too deep to avoid inconvenient removal of the sintered sample; the closed hole 22 cannot be set too shallow, which will be unfavorable for the filling of the sintering raw material.

[0069] In some embodiments of the present invention, as Figure 3 As shown in FIG. 4, the high-throughput mold includes a graphite paper 25, and the graphite paper 25 is arranged at the bottom of the closed hole 22.

[0070] In this embodiment, a graphite paper is placed inside the closed hole 22 before placing the sintering raw material to prevent the sintering raw material 23 from adhering to the porous mold 2.

[0071] In some embodiments of the present utility model, as Figure 1 shown in any one of FIGS. 2 to 4, the lengths of the plurality of sub-punch heads 11 are the same.

[0072] In this embodiment, the lengths of the plurality of sub-punch heads 11 are the same. Thus, the sub-punch heads on the side close to the closed holes 22 can maintain the same height in the horizontal direction, so as to prevent the sub-punch heads 11 from not receiving pressure and pulsed current, and further prevent the sintering raw materials in the closed holes 22 corresponding to the sub-punch heads 11 from being subjected to spark plasma sintering.

[0073] In a second aspect, the present utility model provides a spark plasma sintering device, and the spark plasma sintering device includes the high-throughput mold described in the first aspect above.

[0074] The high-throughput mold of the embodiment of the present utility model is applicable to hot pressing sintering or spark plasma sintering, and can improve the efficiency and sustainability of the hot pressing sintering process or the spark plasma sintering process, thereby accelerating the component screening and optimization of samples. The high-throughput mold provided by the present utility model can ensure the uniformity of the sintered samples even when pulsed current is introduced through the structural arrangement. Therefore, the high-throughput mold is more suitable for spark plasma sintering.

[0075] As Figure 6 shown, the spark plasma sintering device includes a high-throughput mold 3; the spark plasma sintering device includes an upper electrode 51, a lower electrode 52, an upper punch head 41, and a lower punch head 42; wherein 6 is pulsed current.

[0076] Taking the Y 2 O 3 co-stabilized ZrO 2 system as an example, the usage method of the high-throughput mold and the sintering device provided by the present utility model will be further described.

[0077] The spark plasma sintering device uses a 2HSPS-45000-60AT type spark plasma hot sintering device produced by Shenzhen Xingyuan Spark Plasma Technology Co., Ltd.; the sintering raw materials Y 2 O 3 powder and ZrO 2 powder are both provided by Sinopharm Chemical Reagent Co., Ltd. Among them, in the Y 2 O 3 co-stabilized ZrO 2 with different component ratios, the addition amounts of Y 2 O 3 are 7wt%, 15wt%, 25wt%, 35wt%, 45wt%, 55wt%, and 65wt% respectively, and Y 2 O 3The powder particle size distribution is D10 = 2.828 μm, D50 = 9.165 μm, or D90 = 19.80 μm, ZrO 2 The powder particle size distribution is D10 = 1.869 μm, D50 = 8.719 μm, or D90 = 23.34 μm.

[0078] The method for using a high-throughput mold includes:

[0079] S1, Mix all the raw materials to be sintered for loading;

[0080] By wet ball milling, Y with different component ratios 2 O 3 powder and ZrO 2 powder are uniformly mixed to obtain a mixed powder, which is the sintering raw material 23; among them, a 5L polytetrafluoroethylene ball milling tank is selected for the ball milling tank; the ball milling beads can be selected in three sizes: large, medium, and small. The large size is 8 - 10 mm, the medium size is 4 - 7 mm, and the small size is 2 - 3 mm. The mass ratio of large grinding balls, medium grinding balls, and small grinding balls is 2:3:5; the ball milling medium is anhydrous ethanol with a concentration of 99.9% and a density of 0.79 g / mL; the mass ratio of ball milling beads, mixed powder, and ball milling medium is 5:1:(1 - 2); the ball mill used is the GMS-20-8 double-layer drum type ball mill produced by Changsha Miqi Instrument and Equipment Co., Ltd.

[0081] S2, Use the double-layer structure high-throughput mold as Figure 2 shown. First, load graphite paper 25 into the closed holes 22 to prevent the mixed powder from adhering to the high-throughput mold during high-temperature sintering;

[0082] S3, Put the mixed powder into the closed holes 22 in the upper layer respectively, and mark each sample. If the number of samples is not enough to fill all the closed holes 22, then give priority to filling the closed holes 22 at the central position;

[0083] S4, Adjust the (unloaded) height of the closed holes 22 in the upper layer to be on the same horizontal plane through the spacer blocks 24, so that the sub-punch 11 in the upper layer vertically covers above each spacer block 24;

[0084] S5, Flip the porous mold 2, put the mixed powder into the closed holes 22 in the lower layer respectively, and mark each sample. If the number of samples is not enough to fill all the closed holes 22, then give priority to filling the closed holes 22 at the central position;

[0085] S6, Adjust the (unloaded) height of the closed holes 22 in the lower layer to be on the same horizontal plane through the spacer blocks 24, so that the sub-punch 11 in the lower layer vertically covers above each spacer block 24, obtaining a high-throughput mold filled with samples;

[0086] S7. Place the high-throughput mold obtained in S6 into the spark plasma sintering chamber, and set the sintering process as follows: sintering temperature 1500 °C, sintering pressure 50 MPa, and holding time 5 min;

[0087] S8. After 5 min, take out the sintered samples from the high-throughput mold in sequence, grind off the graphite paper adhered to the surface, and collect them for standby to conduct material screening and composition optimization.

[0088] In the description of this specification, the description with reference to terms such as "one embodiment", "some embodiments", "schematic embodiments", "examples", "specific examples", or "some examples", etc. means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

[0089] Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art can understand that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the claims and their equivalents.

Claims

1. A high-throughput mold for spark plasma sintering, characterized in that: The high-throughput mold includes at least one press head and a porous mold; The porous mold includes one or two open holes, and the open holes are provided with a plurality of closed holes; the closed holes are holes that do not penetrate, and the closed holes are provided along the vertical direction of the porous mold, and the apertures of the plurality of closed holes are the same, and the closed holes are used to place sintering raw materials, and the sintering raw materials include block raw materials, lamellar raw materials and powder-block raw materials; The pressure head is provided with a plurality of sub-pressure heads, and the sub-pressure heads correspond to the plurality of closed holes one by one; the pressure head includes a large pressure head; The closed holes opened on one of the two open hole surfaces are arranged alternately or aligned with the closed holes opened on the other open hole surface; The high-throughput mold comprises a pad, which covers the sintering raw material and is located on a side close to the sub-pressing head.

2. The high-throughput mold according to claim 1, characterized in that: The closed pores opened on the open pore surface are evenly distributed.

3. The high-throughput mold according to claim 2, characterized in that: The closed cells are arranged and distributed orthogonally.

4. The high-throughput mold according to claim 2, characterized in that: The closed cells are closely packed.

5. The high-throughput mold according to claim 1, characterized in that: The high-throughput mold includes graphite paper, and the graphite paper is arranged at the bottom of the closed cells.

6. The high-throughput mold according to claim 1, characterized in that: The lengths of the plurality of sub-pressure heads are consistent.

7. A spark plasma sintering device, characterized in that: The spark plasma sintering equipment comprises the high-throughput mold as described in any one of claims 1 to 6.

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