CN113851255A - High-insulation easy-rheological thermocouple boron nitride-based filling material and filling method - Google Patents
High-insulation easy-rheological thermocouple boron nitride-based filling material and filling method Download PDFInfo
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- CN113851255A CN113851255A CN202111049166.9A CN202111049166A CN113851255A CN 113851255 A CN113851255 A CN 113851255A CN 202111049166 A CN202111049166 A CN 202111049166A CN 113851255 A CN113851255 A CN 113851255A
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- 239000000463 material Substances 0.000 title claims abstract description 58
- 238000011049 filling Methods 0.000 title claims abstract description 55
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 40
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000009413 insulation Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000011521 glass Substances 0.000 claims abstract description 36
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000011812 mixed powder Substances 0.000 claims description 16
- 239000010935 stainless steel Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical group CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 229940116411 terpineol Drugs 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 12
- 239000007791 liquid phase Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000003566 sealing material Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000001125 extrusion Methods 0.000 abstract description 2
- 239000000395 magnesium oxide Substances 0.000 description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
- 239000006004 Quartz sand Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009529 body temperature measurement Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000005678 Seebeck effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/08—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances quartz; glass; glass wool; slag wool; vitreous enamels
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/025—Other inorganic material
Abstract
The invention relates to the field of boron nitride-based filling materials, in particular to a high-insulation and rheologic thermocouple boron nitride-based filling material and a filling method. The material comprises the following raw materials in parts by weight: 80-90 parts of boron nitride, 10-20 parts of glass micro powder and 1-2 parts of binder. The rheological property of the filling material is improved by adding the glass micro powder. The h-BN ceramic block body formed by extrusion molding is used as a possible filling material for thermocouple application, has a composite structure of a layered ceramic main body and a glass liquid phase surface in a working state, and can meet multiple requirements of a sealing material such as high-temperature insulation, structural stability and interface lubricity. The filling material and the preparation method have the advantages of low cost, simple preparation and stable and reliable quality, and are suitable for industrialized batch preparation.
Description
Technical Field
The invention relates to the field of boron nitride-based filling materials, in particular to a high-insulation and rheologic thermocouple boron nitride-based filling material and a filling method.
Background
The thermocouple sensor is the most commonly used contact temperature measuring device in the industry, can directly convert heat energy into an electric signal, outputs a direct current voltage signal, and can quickly display, record and transmit temperature data. From the research trend at home and abroad, the high-precision fast-response superfine thermocouple is the mainstream of the current research, and has the advantages of stable performance, large temperature measurement range, capability of remotely transmitting signals and the like, simple structure and convenient use. The thermocouple mainly comprises a thermocouple wire, an insulating filling material, a protective sleeve and a junction box, the test temperature is between 0 and 1800 ℃, and the dual functions of sealing and insulating are realized between two thermocouple wire electrodes and between the thermocouple wire and the protective sleeve by applying the high-insulating filling material. The thermocouple is used for the temperature measurement port at its thermocouple silk both ends in normal atmospheric temperature environment in the course of the work, be called the cold junction, heat at thermocouple silk splice point department, utilize the seebeck effect, the cold junction of thermocouple silk produces the temperature difference and then produces the potential difference with the hot junction of splice point department, because the seebeck coefficient of two thermocouple silk metal materials is different, lead to the potential difference to distinguish, calculate according to the linear relation of thermoelectric effect and draw thermocouple silk cold junction and hot junction temperature difference through measuring two thermocouple silk cold junction potential differences, and then record the detected object temperature. To ensure proper operation of the thermocouple, the filler material must provide sufficient insulation to prevent the two thermocouple wires from contacting and causing a short circuit. In addition, the filling material also needs to have the characteristics of resistance wire obstruction, thermal stress absorption, moisture resistance, low manufacturing cost, high reliability and the like.
At present, the filling materials of the thermocouple are mainly divided into three types, namely powdered quartz sand, MgO powder and glass powder. The powdered quartz sand has high temperature resistance, corrosion resistance and high insulating property and is applied to a thermocouple as a filling material, but the powdered quartz sand has a small thermal expansion coefficient and is not easy to match with a thermocouple filling part so as to cause deformation. In addition, when the operating temperature of the thermocouple rises by 100 ℃, the insulation resistance thereof is reduced by an order of magnitude, and when the temperature of the middle part of the thermocouple is higher, leakage current is generated, so that shunt error exists in the output potential of the thermocouple, and the final measurement error is caused. Compared with the powder quartz sand filling material, the MgO powder has good insulativity, electrical strength, thermal conductivity, heat resistance and vibration resistance, the electrical conductivity is less than 10-14 mu s/cm, and the MgO powder reaches a compact state. The thermal expansion coefficient matching between the MgO powder and the part to be filled is better, so the MgO powder is a more filling material used in the thermocouple at present. However, the MgO powder easily absorbs moisture and carbon dioxide in the air, which causes a decrease in insulation resistance and thus decreases thermocouple accuracy. In addition, in the process of testing the thermocouple at a high temperature of over 1000 ℃ for a long time, the MgO filled powder is converted into crystals, the accuracy of the thermocouple detection temperature is affected, and the high-temperature insulation effect is not ideal, so that the effective insulation in the thermocouple operation process is difficult to ensure.
Disclosure of Invention
In order to overcome the defect that the existing filling material cannot ensure effective insulation in the thermocouple operation process, the invention provides a high-insulation and rheologic thermocouple boron nitride-based filling material and a filling method.
The technical scheme adopted by the invention for solving the technical problems is as follows: a high-insulation and rheologic thermocouple boron nitride-based filling material comprises the following raw materials in parts by weight:
80-90 parts of boron nitride, 10-20 parts of glass micro powder and 1-2 parts of binder.
According to another embodiment of the invention, the glass powder further comprises 85 parts of boron nitride, 15 parts of glass micropowder and 1.5 parts of binder.
According to another embodiment of the invention, the glass powder further comprises 80 parts of boron nitride, 10 parts of glass micropowder and 1 part of binder.
According to another embodiment of the invention, the glass powder further comprises 90 parts of boron nitride, 20 parts of glass micropowder and 2 parts of binder.
According to another embodiment of the invention, the boron nitride is h-BN layered structure micropowder.
According to another embodiment of the present invention, it is further comprised that the binder is terpineol.
A filling method of a high-insulation rheologic thermocouple boron nitride-based filling material comprises the following specific steps:
(a) uniformly mixing boron nitride, glass micropowder and a binder in proportion to obtain mixed powder;
(b) grinding the mixed powder in one step;
(c) weighing the ground mixed powder, and putting the powder into a tablet press to prepare a filling material block;
(d) and (3) penetrating the combination of the filling material block and the thermocouple wire into a stainless steel sleeve, and setting a temperature rise program for heat treatment drawing.
According to another embodiment of the present invention, further comprising the step of further grinding the mixed powder is performed by an agate mortar.
The invention has the beneficial effect that the rheological property of the filling material is improved by adding the glass micro powder. The h-BN ceramic block body formed by extrusion molding is used as a possible filling material for thermocouple application, has a composite structure of a layered ceramic main body and a glass liquid phase surface in a working state, and can meet multiple requirements of a sealing material such as high-temperature insulation, structural stability and interface lubricity. The filling material and the preparation method have the advantages of low cost, simple preparation and stable and reliable quality, and are suitable for industrialized batch preparation.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a graph of the trend of the resistivity of the filler material of the present invention as a function of temperature at different operating temperatures;
fig. 2 is an XRD phase structure analysis chart of boron nitride after high temperature treatment.
Detailed Description
FIG. 1 is a graph of the trend of the resistivity of the filler material of the present invention as a function of temperature at different operating temperatures; fig. 2 is an XRD phase structure analysis chart of boron nitride after high temperature treatment.
The first embodiment is as follows:
(a) uniformly mixing 85 parts of boron nitride, 15 parts of glass micropowder and 1.5 parts of binder to obtain mixed powder;
(b) grinding the mixed powder in one step;
(c) weighing the ground mixed powder, and putting the powder into a tablet press to prepare a filling material block;
(d) and (3) penetrating the combination of the filling material block and the thermocouple wire into a stainless steel sleeve, and setting a temperature rise program for heat treatment drawing.
Example two: uniformly mixing 80 parts of boron nitride, 10 parts of glass micropowder and 1 part of binder to obtain mixed powder;
(a) grinding the mixed powder in one step;
(c) weighing the ground mixed powder, and putting the powder into a tablet press to prepare a filling material block;
(d) and (3) penetrating the combination of the filling material block and the thermocouple wire into a stainless steel sleeve, and setting a temperature rise program for heat treatment drawing.
Example three:
(a) 90 parts of boron nitride, 20 parts of glass micropowder and 2 parts of binder;
(a) grinding the mixed powder in one step;
(c) weighing the ground mixed powder, and putting the powder into a tablet press to prepare a filling material block;
(d) and (3) penetrating the combination of the filling material block and the thermocouple wire into a stainless steel sleeve, and setting a temperature rise program for heat treatment drawing.
The boron nitride is h-BN layered structure micro powder, the size of the h-BN layered structure micro powder is 5-8 mu m, and the Coefficient of Thermal Expansion (CTE) is 10.3 multiplied by 10 < -6 > K < -1 >. The glass powder is selected to have a coefficient of thermal expansion matched to the particle size, such as the SiO2-Na2O-K2O3 system.
As shown in the attached drawings 1 and 2, the h-BN layered structure micropowder is a polar covalent bond system, intermolecular force exists between the lamellae, and free electrons do not exist in the h-BN crystalline layer structure, so the h-BN layered structure micropowder is not conductive. Therefore, the h-BN micro powder is used as the thermocouple filling material, and the high insulation property is achieved in the process from low temperature to high temperature. In addition, in the atomic crystal, the melting point of a substance is inversely proportional to the atomic radius and the bond length, and the bond energy is larger and less prone to break as the covalent bond is shorter, so that the melting point of the boron nitride crystal is higher, and the layered structure can be maintained to effectively fill the gap between the thermocouple wire and the stainless steel sleeve.
The h-BN material has a layered structure, so that powder materials of the h-BN material have good rheological properties in different temperature ranges, the h-BN material is softened when the working temperature is over 500 ℃, and when the temperature reaches the melting point of B2O3, namely 577 ℃, a B2O3 liquid-phase film is formed on the surface of the h-BN material, so that the h-BN material has a good infiltration effect on adjacent thermocouple wires and metal sleeves, reliable filling is realized, and the rheological properties of the h-BN-based sealing material are improved. Below 1000 ℃, the B2O3 liquid film can prevent oxygen from diffusing into the h-BN and the surface of the thermocouple wire from the air, so that an effective oxygen diffusion barrier layer is formed, and further oxidation of the thermocouple wire filled in the h-BN ceramic is prevented. In addition, the softened glass layer can reduce the deformation friction resistance between the thermocouple metal wire and the ceramic powder, and is favorable for the uniform deformation of the superfine thermocouple metal wire.
The h-BN is a hydrophobic material, and a certain amount of glass powder is added into the h-BN differential to enhance the internal bonding force of the h-BN. When the thermocouple works in a high-temperature state, the h-BN ceramic micro powder is coated and sintered together by the glass micro powder, so that the phenomenon of reduction of insulation resistance caused by moisture absorption of the conventional magnesium oxide powder can be effectively avoided. In addition, the boron nitride-based insulating material is prepared by compounding the glass and the boron nitride powder in a certain proportion, so that the rheological behavior among the metal thermocouple wire, the filling powder and the alloy sleeve of the thermocouple can be effectively regulated and controlled, and the high-quality molding of the superfine thermocouple is realized.
In a high-temperature working state of the thermocouple wire, a B2O3 liquid-phase film can be generated on the surface of the boron nitride-based filling material, the high-viscosity B2O3 liquid-phase film can infiltrate the surface of the thermocouple wire or the stainless steel sleeve, good interface connection and filling are realized, and accordingly the insulativity of the h-BN-based filling material is improved. In addition, after the glass micro powder in the filling material is melted and coated with the ceramic powder in a working state, the phenomenon of insulation resistance reduction caused by moisture absorption of the conventional magnesium oxide powder is avoided, and the rheological property of the filling material is improved. The softened glass layer reduces the deformation frictional resistance between the thermocouple wire and the ceramic powder, and is beneficial to the uniform deformation of the superfine thermocouple wire.
The glass micro powder can be softened at the working temperature of the thermocouple wire, and under the action of external pressure, liquid phase generated by the h-BN ceramic micro powder is tightly combined with glass, so that the fracture energy of the sealing material is improved; on the other hand, the glass and the h-BN ceramic micro powder interface are diffused and even reacted, so that the bonding strength between the glass and the ceramic particles is improved, and the mechanical property of the material is further improved. If an excessive amount of fine glass powder is added, problems of glass state such as easy devitrification of glass, generation of cracks in a cooling-heating cycle, and the like are revealed.
Claims (8)
1. A high-insulation rheologic thermocouple boron nitride-based filling material is characterized by comprising the following raw materials in parts by weight:
80-90 parts of boron nitride, 10-20 parts of glass micro powder and 1-2 parts of binder.
2. The high-insulation rheopectic thermocouple boron nitride-based filling material according to claim 1, wherein the boron nitride is 85 parts, the glass micropowder is 15 parts, and the binder is 1.5 parts.
3. The high-insulation rheopectic thermocouple boron nitride-based filling material according to claim 1, wherein the boron nitride is 80 parts, the glass micropowder is 10 parts, and the binder is 1 part.
4. The high-insulation rheopectic thermocouple boron nitride-based filling material according to claim 1, wherein the boron nitride is 90 parts, the glass micropowder is 20 parts, and the binder is 2 parts.
5. The high-insulation rheopectic thermocouple boron nitride-based filling material according to claim 1, wherein the boron nitride is h-BN layered structure micropowder.
6. A high dielectric, rheologically easy thermocouple boron nitride based filler material as in claim 1, wherein said binder is terpineol.
7. The method for filling the high-insulation rheopectic thermocouple boron nitride-based filling material according to any one of claims 1 to 6, which is characterized by comprising the following steps:
(a) uniformly mixing boron nitride, glass micropowder and a binder in proportion to obtain mixed powder;
(b) grinding the mixed powder in one step;
(c) weighing the ground mixed powder, and putting the powder into a tablet press to prepare a filling material block;
(d) and (3) penetrating the combination of the filling material block and the thermocouple wire into a stainless steel sleeve, and setting a temperature rise program for heat treatment drawing.
8. The high insulation rheopectic thermocouple boron nitride-based filler material according to claim 7, wherein the mixed powder is ground in one step by means of an agate mortar.
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1095812A (en) * | 1964-09-10 | 1967-12-20 | Engelhard Ind Inc | Thermocouple assembly |
US4590326A (en) * | 1984-06-14 | 1986-05-20 | Texaco Inc. | Multi-element thermocouple |
CN1229189A (en) * | 1998-01-12 | 1999-09-22 | 株式会社五十铃硅酸盐研究所 | Electric thermo-couple for measuring temp. of metal solution |
WO2011102810A1 (en) * | 2010-02-19 | 2011-08-25 | Hidria Aet Druzba Za Proizvodnjo Vzignih Sistemov In Elektronike D.O.O. | Process of manufacturing temperature probes |
US20150211942A1 (en) * | 2012-10-19 | 2015-07-30 | Okazaki Manufacturing Company | Cryogenic temperature measuring resistor element |
CN106683748A (en) * | 2016-12-09 | 2017-05-17 | 东莞珂洛赫慕电子材料科技有限公司 | Environment-friendly low-temperature sintered high-heat-conduction dielectric paste and preparation method therefor |
CN109650355A (en) * | 2017-10-11 | 2019-04-19 | 河北高富氮化硅材料有限公司 | A kind of method of low temperature preparation hexagonal boron nitride |
-
2021
- 2021-09-08 CN CN202111049166.9A patent/CN113851255A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1095812A (en) * | 1964-09-10 | 1967-12-20 | Engelhard Ind Inc | Thermocouple assembly |
US4590326A (en) * | 1984-06-14 | 1986-05-20 | Texaco Inc. | Multi-element thermocouple |
CN1229189A (en) * | 1998-01-12 | 1999-09-22 | 株式会社五十铃硅酸盐研究所 | Electric thermo-couple for measuring temp. of metal solution |
WO2011102810A1 (en) * | 2010-02-19 | 2011-08-25 | Hidria Aet Druzba Za Proizvodnjo Vzignih Sistemov In Elektronike D.O.O. | Process of manufacturing temperature probes |
US20150211942A1 (en) * | 2012-10-19 | 2015-07-30 | Okazaki Manufacturing Company | Cryogenic temperature measuring resistor element |
CN106683748A (en) * | 2016-12-09 | 2017-05-17 | 东莞珂洛赫慕电子材料科技有限公司 | Environment-friendly low-temperature sintered high-heat-conduction dielectric paste and preparation method therefor |
CN109650355A (en) * | 2017-10-11 | 2019-04-19 | 河北高富氮化硅材料有限公司 | A kind of method of low temperature preparation hexagonal boron nitride |
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