JPH0699085A - Ceramic heater/cooler - Google Patents

Abstract

PURPOSE:To enable precise temp. control and programmed temp. managing and control for various purposes by providing a sintered body for which holes, through holes or grooves of desired shapes for supporting a material to be heated or cooled are provided on a plane or the optional surface of the sintered body and disposing heating resistors in the sintered body. CONSTITUTION:This unit is provided with a sintered body having holes, 2, 3, through holes, or grooves of desired shapes on a plane or the optional surface for supporting a material to be heated or cooled, and at least one heating resistor (electrode forming metallized layers on the surfaces 4, 5). Or, a heat- exchanging part for cooling is provided on optional surface or in the sintered body. Since the area being in contact with the material to be heated/cooled is large, conduction of heat is efficiently performed from the heater/cooler to the material to be heated/cooled. Thereby, temp. is rapidly increased or decreased to the objective temp., and good accuracy of temp. distribution is obtd., and precise temp. control can be attained.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a structure of a ceramic heating / cooling device which enables precise temperature control in the fields of medicine, chemistry and biotechnology and has a good temperature distribution accuracy.

[0002]

2. Description of the Related Art In a conventional thermostatic chamber for science and science, since a support for an object to be heated and a heater are separate, temperature distribution accuracy and rapid temperature rise / fall cannot be achieved. It takes a long time to reach a certain temperature, and the response speed is slow when changing the temperature setting. Also, the response to the disturbance was poor and the usability was very poor.

[0003]

SUMMARY OF THE INVENTION The present invention solves the above-mentioned drawbacks of the prior art, quickly raises or lowers the temperature to a predetermined temperature, and quickly responds to temperature changes.
Moreover, the present invention was made to provide a ceramic heating / cooling device capable of performing precise temperature control with fast response to disturbance and good temperature distribution, and rapid heating / cooling.

[0004]

SUMMARY OF THE INVENTION The present invention, which was conceived to solve the above-mentioned problems, provides a sintered body with a hole or groove for supporting an object to be heated, and the sintering. It is characterized in that a sintered body component having good thermal conductivity is used for the body, and a heating resistor mainly composed of metal, conductive ceramics or carbon is embedded inside the sintered body. At the same time, regarding the temperature lowering, a technical method was adopted in which a fin, a honeycomb structure or a pipe having a good heat dissipation property was installed and the surface was cooled by contacting cold air or a refrigerant.

[0005]

[Operation] According to the ceramic heating / cooling device configured as described above, the object to be heated is quickly sintered because it is in contact with the surface, hole or groove provided on the sintered body with good heat conduction. It becomes equal to the temperature of the body heating and cooling device. Further, since the heating resistor is embedded in the sintered body, it is possible to precisely control the temperature. As for the cooling unit, it is possible to install the cooling unit at a low cost by using a material that has good heat dissipation characteristics and is easy to process for the heat radiation unit.

[0006]

Embodiment 1 FIG. 1 shows the appearance of Embodiment 1 of the present invention.
Here, 1 is conductive SiC. Reference numerals 2 and 3 are holes for supporting the object to be cooled. As a method for producing this ceramic substrate, as shown in FIG. 2, a raw material powder mold to which a known sintering aid of conductive SiC raw material powder is added is filled and pressed,
The block 6 is formed. Next, a few holes are formed by a cutting process for supporting the object to be cooled. Next, this is sintered under known sintering conditions. Next, a metallization layer is formed on the surfaces 4 and 5 to serve as electrodes. A characteristic test was performed using the ceramic heating and cooling device manufactured using the above method. Heating and precise temperature control were performed by applying a voltage to the electrodes 4 and 5. The cooling is shown in the schematic diagram of FIG. The block body 8 is cooled by a cold air fan 9. Next, a characteristic test was conducted. A microtube having a thermocouple installed was set in the holes 2 and 3, and a test was conducted under the following conditions. That is, PID control was performed with the thermocouple of the microtube at the position of the hole 2. The initial temperature before operation of the device is 2
The value of the thermocouple of the hole at the position is 17 ° C., and the arbitrary set temperature of the device and the set movable time are programmed as follows. 95 ° C
10 minutes, then 4 ° C. for 60 minutes, then 25 ° C. for 20 minutes. The temperature control and measurement results were set to 95 ° C and the set temperature reached to 95 ° C 8 seconds after the device was operated. Within. The temperature accuracy is within ± 0.1 ° C at the position of each thermocouple with respect to 4 ° C for 60 minutes, the arrival time to the setting 4 ° C is 18 seconds. The thermocouple at the position of the hole 3 with respect to 25 ° C for 20 minutes at the set arrival time of 2 seconds for 2 seconds was operated with temperature accuracy of ± 0.2 ° C and ended. Good test results were obtained. In this embodiment, the block conductive SiC is used, but other conductive ceramics may be used. In this embodiment, the number of holes is two, but the number is not limited to this, and the number of holes can be set freely.

[0007]

Example 2 For the purpose of improving the cooling efficiency in the lower part of the block used in Example 1, unevenness was formed by diamond grinding and the same test as in Example 1 was conducted. Good test results similar to those of Example 1 were obtained.

[0008]

Example 3 An AlN layer was formed on the surface and holes of the block used in Example 2 by CVD to insulate a SiC block from a heated and cooled portion, and a test was conducted. A characteristic test was conducted in the same manner as in Example 1. Good test results similar to those of Example 1 were obtained.

[0009]

Fourth Embodiment As shown in FIG. 5, an adhesive layer 10 is formed on the block of the first embodiment and an aluminum fin 11 is attached. Then, a characteristic test was conducted in the same manner as in Example 1. Good test results similar to those of Example 1 were obtained.

[0010]

Fifth Embodiment As shown in FIG. 6, a cooling pipe 12, 13 was attached to the block of the fourth embodiment instead of the fins, and a test was conducted. A characteristic test was conducted in the same manner as in Example 1.
Good test results similar to those of Example 1 were obtained.

[0011]

Sixth Embodiment As shown in FIG. 7, the block body of the first embodiment is provided with through holes 14, 15, 16 for cooling, and a cooling medium is flown there through for cooling. A characteristic test was conducted in the same manner as in Example 1. Good test results similar to those of Example 1 were obtained.

[0012]

Example 7 Pipes having a honeycomb structure inside the blocks 14, 15 and 16 of Example 6 were installed, and a cooling medium was flowed through them to cool them. A characteristic test was conducted in the same manner as in Example 1. Good test results similar to those of Example 1 were obtained.

[0013]

[Embodiment 8] FIG. 8 shows an appearance of Embodiment 8. Where 17
Is AlN. 18 is a mixed portion of AlN and MoSi ₂ . Numeral 19 is a hole for supporting the object to be heated. 20
Is a metallized part. FIG. 9 shows a cross section taken along the line 9-9 in FIG. As the manufacturing method of this embodiment, the non-conductive raw material powder A is used.
1N and conductive raw material powder AlN 30% and MoSi ₂ 7
The 0% mixture is made into a sandwich structure. That is, as shown in FIG. 10, the mold 21 is filled with 22 of the non-conducting raw material powder AlN. Next, as shown in FIG. 11, a mixture of conductive raw material powder AlN 30% and MoSi ₂ 70% 23
To fill. Next, as shown in FIG. 12, non-conductive raw material powder AlN 24 is filled again, and pressure is temporarily applied by a mold 25 to perform temporary molding. Next, as shown in FIG. 14, holes 28 and 29 for supporting the object to be heated are formed by cutting. Next in FIG.
As shown in FIG. 5, carbon rods 30 and 31 each having a surface coated with a release agent BN or the like are set in the holes, and hot pressing is performed. Figure 1
6 is a cross-sectional view of the portion cut along the AA ′ cross section in FIG. 15 during hot pressing. Here, 35 and 36 are carbon type. 37 is a carbon rod and 34 is a guide hole. An electrode is formed at 20 in FIG. 8 on this sintered body. This was tested in the same manner as in Example 1. Good results similar to those of Example 1 were obtained. In the present embodiment, the number of laminated conductors is one, but the number is not limited to this. Good results are also obtained with a multilayer sandwich structure. Also, the combination of materials is free.

[0014]

Example 9 A fin was attached to the block of Example 8 by the same method as in Example 4, and the same test as in Example 1 was conducted. Good results similar to those of Example 1 were obtained.

[0015]

[Example 10] A cooling pipe similar to that of Example 5 was installed in place of the fins of Example 9, and the same test as that of Example 1 was conducted. Good results similar to those of Example 1 were obtained.

[0016]

[Embodiment 11] The same cooling through holes as in Embodiment 6 were installed in the block of Embodiment 8 and the same test as in Embodiment 1 was conducted. Good results similar to those of Example 1 were obtained.

[0017]

Twelfth Embodiment FIG. 17 shows the appearance of this embodiment. Here, 38 is an AlN block body, and 39 and 40 are through holes for supporting the object to be heated. AA 'is shown in FIG. 4 here
2 is AlN and 43 is carbon. As a method of manufacturing this block body, a raw tape of AlN is made as shown in FIG. Here, 43, 44, and 46 are raw tapes of AlN, and 43 is a carbon paste, and is printed by a method such as screen printing. Then, these three sheets are laminated and sintered. As shown in FIG. 17, metallization is performed to form electrodes 41. This was tested in the same manner as in Example 1. Good results similar to those of Example 1 were obtained.
Here, only three layers are stacked, but the number of layers is not limited to this. The number of layers can be freely set as needed.

[0018]

[Embodiment 13] FIG. 20 shows the appearance of Embodiment 13. Here, 47 is a block body. 48, 49, 50, 51
Is a hole for supporting a test tube. 52 is an electrode. Figure 2
FIG. 1 shows a cross section taken along the line AA ′ of FIG. Where 53 is Al
There are N. 54 is TiN. As a method of manufacturing this block body, first, a green sheet of TiN is prepared.
It shows in FIG. This green sheet is punched into a shape as shown in FIG. The punched sheet is 55.
Next, as shown in FIG. 24, AlN powder 57 is applied to the mold 56.
To fill. As shown in FIG. 25, punched TiN 55 is set on this powder 57. Next, as shown in FIG. 26, AlN powder is filled again. Then, it is pressure-molded. Next, hot press sintering is performed, the end face is ground, TiN is taken out, and the portion is metallized to form an electrode. The same test as in Example 1 was performed. Good test results similar to those of Example 1 were obtained.

[0019]

[Embodiment 14] FIG. 27 shows an appearance of Embodiment 14. Here, 58 is a block body, and 59 and 60 are holes for supporting a test tube. Reference numerals 62 and 63 are observation through holes for observing the sample in the test tube by optical measurement or the like. Reference numerals 64, 65 and 66 are through holes for passing the refrigerant. FIG. 28 shows a cross section taken along the line AA ′ of FIG. With such a device, it is possible to measure the current state from the observation through hole while maintaining the temperature control of the sample.

[0020]

Fifteenth Embodiment FIG. 29 shows the appearance of the fifteenth embodiment. Here, 68 is AlN. 69 is an electrode. Reference numeral 70 is a cooling through hole through which a coolant flows. FIG. 30 shows a cross section taken along the line AA ′ of FIG. Here, 71 is tungsten. Figure 31
FIG. 29 shows an actual use state as seen from the BB ′ cross section of FIG. Here, 72 is a sample holding container, and 73 is a hole for sample injection. Reference numeral 74 is a heating resistor, and 75 is a cooling through hole. Now put the same amount of pure water in each hole,
The temperature control method was the same as in Example 1. The temperature was controlled by a thermocouple placed in the hole. After that, the same test as in Example 1 was performed. The same good results as in Example 1 were obtained,
Only the temperature accuracy at each hole was within ± 1 ° C. In this embodiment, AlN is used for the heating / cooling body and tungsten is used for the heating resistor. Further, for cooling, the cooling medium is flowed through the cooling through hole, but the cooling method is not limited to this. The combination of the body material, the heating resistor material and the cooling method is free.

[0021]

16th Embodiment FIG. 32 shows the appearance of the 16th embodiment. Here, 76 is a main body using AlN. 77 is an electrode,
Reference numeral 78 is a hole, and 79 is a cooling fin. 32 in FIG.
The actual use condition seen from the AA ′ cross section of FIG. Where 8
0 is a sample holding container. 81 is a hole for sample injection. Reference numeral 82 is a heating resistor. Example 16
The same test was performed. However, for cooling, cold air was applied to the cooling fins from the bottom. Good results similar to those of Example 15 were obtained.

[0022]

As described above, according to the present invention, a metal or conductive ceramic heating element is embedded in a sintered body having good heat conduction, and the heat dissipation is good, and Since the cooling part made of a material that can be easily processed is provided, an inexpensive cooling part is possible. Since the area in contact with the object to be heated is wide, heat can be efficiently conducted from the heating cooler to the object to be heated. Therefore, the temperature can be raised and lowered quickly with respect to the set temperature, and the temperature distribution accuracy is improved, enabling precise temperature control. Therefore, in the conventional technology,
Precise temperature control of various temperature patterns has become possible, new applications have opened up, complicated temperature program control has become possible, and new operation methods have become possible in the biotechnology and chemistry fields. .

[Brief description of drawings]

FIG. 1 Appearance of Example 1

[Figure 2] Generating body

[Fig. 3] A state in which holes are formed in the generative body.

FIG. 4 is a schematic diagram of cooling

FIG. 5 Appearance of Example 4

FIG. 6 Appearance of Example 5

FIG. 7 Appearance of Example 6

FIG. 8 Appearance of Example 8

9 is a cross section taken along the line AA ′ of FIG.

FIG. 10 shows a mold filled with raw material powder.

FIG. 11 shows a mold filled with raw material powder.

[Fig. 12] Molded into a sandwich

FIG. 13: Temporary molding of sandwich structure

[Fig. 14] A hole formed in a temporary molded body

FIG. 15 shows a state where a carbon rod is set on a temporary molded body.

FIG. 16 is a cross section at the time of hot pressing

FIG. 17 Appearance of Example 12

18 is a cross section taken along line AA ′ of FIG.

FIG. 19: Raw tape before lamination

FIG. 20 Appearance of Example 13

21 is a cross section taken along the line AA ′ of FIG.

FIG. 22: Green sheet of conductive ceramic

FIG. 23: Punched green sheet

FIG. 24 shows a state in which a raw material powder of insulating ceramic is filled in a mold.

FIG. 25 shows a state in which a conductive ceramic green sheet is set in the mold.

FIG. 26 shows a state in which a mold is filled with a conductive ceramic and an insulating ceramic raw material.

FIG. 27 Appearance of Example 14

28 is a cross section taken along line AA ′ of FIG. 27.

FIG. 29 Appearance of Example 15

30 is a cross section taken along line AA ′ of FIG. 29.

[Fig. 31] Cross-section in actual use

32 is an appearance of Example 16 FIG.

FIG. 33 is a cross section of an actual use state

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Ceramic base 2, 3 Holes for supporting heated object to be heated 4, 5 Electrode 6 Generation type body 7 State in which holes are formed in generation type body 8 Ceramic base body 9 Cool air fan 10 Adhesive layer 11 Cooling fins 12, 13 Cooling pipe 14, 15, 16 Cooling Through Hole 17 Insulating Ceramic Substrate 18 Conductive Ceramic Substrate 19 Heated Material Support Hole 20 Electrode 21 Mold 22, Insulating Ceramic Raw Material Powder 23 Conductive Ceramic Raw Material Powder 24 Insulating Ceramic Raw Material Powder 25 Mold 26 Insulating raw material 27 Conductive raw material 28, 29 Heated object supporting hole 30, 31 Carbon 32 Insulator part 33 Conductor part 34 Guide hole 35, 36, 37 Carbon 38 Ceramic substrate 39, 40 Heated cooling Through hole for supporting objects 41 Electrode 42 Ceramic substrate 43 Heating resistor 44, 46 Generation type body 45 holes 47 ceramic bases 48, 49, 50, 51 holes for supporting objects to be heated 52 electrodes 53 ceramic bases 54 heating resistors 55 heating resistors green 58 ceramic bases 59, 60 holes for supporting objects to be heated 61 electrodes 62, 63 Observation through holes for measurement 64, 65, 66 Cooling through holes 67 Heating resistor 68 Ceramic substrate 69 Electrode 70 Cooling through hole 71 Heating resistor 72 Sample holder 73 Sample hole 74 Heating resistor 75 Cooling through hole 76 Ceramic substrate 77 Electrode 78 Hole 80 Sample holder 81 Sample hole 82 Heating resistor

Continuation of the front page (31) Priority claim number Japanese Patent Application No. 4-213145 (32) Priority Day 4 (1992) July 2 (33) Country of priority claim Japan (JP) (31) Priority claim number Special Wishhei 4-247044 (32) Priority date Hei 4 (1992) August 3 (33) Priority claiming country Japan (JP)

Claims (23)

[Claims] 1. A sintered body having a hole or a through hole or groove having a desired shape for supporting an object to be heated, which is planar or has an arbitrary surface, and one or more heating resistors in the sintered body. Ceramic heating and cooling device that is characterized. 2. The ceramic heating / cooling device according to claim 1, wherein a heat exchange portion for cooling is provided on an arbitrary surface or inside of the sintered body. 3. The ceramic heating / cooling device according to claim 1, wherein the cooling heat exchange portion has a flat surface or unevenness on any surface. 4. The ceramic heating / cooling device according to claim 1, wherein the cooling heat exchange portion has a structure in which a cooling fin, a honeycomb structure, or a pipe is attached to an arbitrary surface. 5. The ceramic heating and cooling device according to claim 1, wherein the cooling heat exchange portion has a through hole for cooling in which a hollow, pipe or honeycomb structure is installed in the sintered body. 6. The structure according to claim 1, wherein an arbitrary portion of the sintered body is provided with an observation hole or an optical path structure for optical measurement of the object to be heated to be cooled having a desired shape. Ceramic heating and cooling device. 7. The ceramic heating / cooling device according to claim 6, wherein the observation hole or the optical path is a through hole in the sintered body. 8. The ceramic heating and cooling device according to claim 6, wherein the observation hole or the optical path is a translucent ceramic in a sintered body. 9. The ceramic heating / cooling device according to claim 6, wherein the observation hole or the optical path is a transparent glass in the sintered body. 10. The ceramic heating / cooling device according to claim 6, wherein the observation hole or the optical path is a transparent resin in the sintered body. 11. The sintered body has a thermal conductivity of 10 W / m ° K.
The ceramic heating and cooling device according to claim 1, characterized in that it is the above. 12. The ceramic heating / cooling device according to claim 1, wherein the sintered body material is an insulating ceramic. 13. The ceramic heating / cooling device according to claim 1, wherein the sintered body material is a conductive ceramic, and the sintered body itself generates heat when energized. 14. The ceramic heating / cooling device according to claim 1, wherein the heating resistor is an inorganic conductor material. 15. The ceramic heating / cooling device according to claim 14, wherein the heating resistor material is a metal. 16. The ceramic heating / cooling device according to claim 14, wherein the heating resistor material is a conductive ceramic. 17. The ceramic heating / cooling device according to claim 14, wherein the heating resistor material is carbon. 18. The main component of the sintered body is -60.degree. C. to 300.degree.
Claim 1 is characterized in that it is composed of a sintered body made of a conductive ceramics having a thermal conductivity of 10 W / m ° K or more in the above range, and the conductive ceramics also serves as a heating resistor. The ceramic heating and cooling device according to the item. 19. The main component of the sintered body is SiC, TiN, Mo.
The ceramic according to claim 1, characterized in that the ceramic is composed of a sintered body made of at least one kind of conductive ceramics such as Si ₂ , ZrB ₂ and WC, and the heating resistor also serves as the heating resistor. Heating cooler. 20. The main component of the sintered body is -60.degree. C. to 300.degree.
, The thermal conductivity of which is 10 W / m ° K or higher, and the heating resistor is made of conductive ceramics and the thermal conductivity of which is 10 W / m ° K or higher. The ceramic heating / cooling device according to claim 1, wherein the ceramic heating / cooling device is composed of a conductive ceramic material containing the same material as described in (1) above. 21. The main component of the sintered body is made of at least one ceramics such as SiC, MgO, S ₃ N ₄ , and Al ₂ O ₃ which are insulative with AlN, and the heating resistor is made of a conductive material. SiC, TiN, MoSi ₂ , ZrB ₂ ,
WC, RCrO ₃ or other conductive ceramics or a conductive material component made of one or more kinds of carbon and the same material as the main component of the sintered body composed of ceramics having a thermal conductivity of 10 W / m ° K or higher are mixed. The ceramic heating / cooling device according to claim 1, wherein the ceramic heating / cooling device is composed of a substance containing a conductive ceramics as a main component. 22. The main component of the sintered body is -60.degree. C. to 300.degree.
In the range, the thermal conductivity is 10 W / m ° K or more, and the heat-generating resistor has a specific resistance value of 10 ⁵ Ω.
The ceramic heating / cooling device according to claim 1, wherein the heating / cooling device is made of a material having Cm or less. 23. The main component of the sintered body is a specific resistance value of 10 ⁷ ΩC.
m or more SiC, MgO, Si ₃ N ₄ , Al ₂ O ₃ , A
The heating resistor is made of a sintered body composed of at least one component selected from 1N and BeO ₂ , and the heating resistor is made of metal such as tungsten, molybdenum, rhenium, or platinum, TiN,
MoSi ₂ , ZrB ₂ , WC, TaC, RCrO ₃ is a substance containing at least one or more kinds of conductive ceramics such as silicon carbide having a volume resistivity of 10 ⁷ ΩCm or less, or carbon. The ceramic heating and cooling device according to claim 1, characterized in that it is configured.