CN113088869A - Preparation method of tantalum carbide sheet - Google Patents
Preparation method of tantalum carbide sheet Download PDFInfo
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- CN113088869A CN113088869A CN202110347357.7A CN202110347357A CN113088869A CN 113088869 A CN113088869 A CN 113088869A CN 202110347357 A CN202110347357 A CN 202110347357A CN 113088869 A CN113088869 A CN 113088869A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
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Abstract
A preparation method of tantalum carbide sheets belongs to the technical field of preparation of tantalum carbide materials. The technical problem to be solved by the invention is the problem of material surface smoothness. The method comprises the steps of vertically placing silicon nitride wedges on the inner wall of a graphite heater, placing 1 silicon nitride wafer among 3 wedges, placing the silicon nitride wafers on the inner bottom surface of the graphite heater, placing 1 graphite powder wafer and 1 tantalum wafer on the silicon nitride wafers in sequence, placing 1 graphite powder wafer and 1 tantalum wafer above the tantalum wafers, placing 6 graphite powder wafers and 5 tantalum wafers together in sequence, placing 1 silicon nitride wafer, placing the graphite heater integrally in an induction heating furnace after screwing an upper cover of the graphite heater, raising the temperature to 1800 ℃ within 4 hours after vacuumizing, filling protective gas into the furnace to enable the furnace pressure to reach 750Torr, preserving heat for 1 hour, and raising the furnace temperature to 2100 ℃ for reaction. The method is used for growing the tantalum carbide sheet.
Description
Technical Field
The invention belongs to the technical field of preparation of tantalum carbide materials; in particular to a preparation method of a tantalum carbide sheet.
Background
The aluminum nitride belongs to the third generation semiconductor material, and has the characteristics of high forbidden band width, high thermal conductivity, high electron drift rate, high chemical stability and the like. Because of good physical properties, the material has wide application prospects in the aspects of high-temperature, high-frequency and high-power devices, deep ultraviolet photoelectronic devices and the like.
A commonly used method for producing aluminum nitride single crystal is a physical vapor transport method. In a specific experiment, if an induction heating furnace is used to grow an aluminum nitride single crystal, a tantalum crucible and a tantalum sheet are generally used as a crucible combination for crystal growth. Because the temperature used when the aluminum nitride grows the crystal is high, the aluminum nitride raw material can decompose the gaseous component, the crucible made of pure tantalum material can deform at high temperature, and can react with the gaseous component of the aluminum nitride raw material to influence the crystal growth result, so the tantalum crucible is carbonized before the crystal growth, and the tantalum material is changed into a more stable tantalum carbide material. The ordinary carbonization process is to put the tantalum sheet into graphite powder, put into graphite crucible, heat up the carbonization in high temperature induction heating stove, because graphite powder thickness is inhomogeneous, can make the tantalum sheet carbonization rear surface unevenness, influence long brilliant messenger and use.
Disclosure of Invention
The invention aims to provide a preparation method of a tantalum carbide sheet with a smooth surface.
The invention is realized by the following technical scheme:
a preparation method of tantalum carbide sheets comprises the following steps:
step 4, charging, namely vertically placing silicon nitride wedges against the inner wall of a graphite heater, wherein the distance between every two silicon nitride wedges is equal, placing 1 silicon nitride wafer between 3 wedges, placing the silicon nitride wafers on the inner bottom surface of the graphite heater, placing 1 graphite powder wafer and 1 tantalum wafer on the silicon nitride wafers in sequence, then placing 1 graphite powder wafer and 1 tantalum wafer above the tantalum wafers, placing 6 graphite powder wafers and 5 tantalum wafers in sequence, then placing 1 silicon nitride wafer above the graphite powder wafers, and screwing the upper cover of the graphite heater;
step 5, putting the graphite heater installed in the step 4 into an induction heating furnace integrally, and vacuumizing to enable the vacuum degree to reach 10-4After Pa, the temperature was raised to 1800 ℃ within 4 hours, and then a protective gas was introduced into the furnaceHeating the furnace to reach 750Torr, keeping the temperature for 1h, then heating the furnace to 2100 ℃, keeping the temperature and pressure for reaction for 20h, then cooling, and heating the furnace to 1000 ℃ within 4h, and finishing the reaction;
and 6, opening the furnace to take out the graphite heater, taking out the tantalum sheet after reaction, and respectively cleaning the tantalum sheet by using absolute ethyl alcohol and acetone in an ultrasonic cleaning machine to obtain the tantalum carbide sheet.
According to the preparation method of the tantalum carbide sheet, the diameter of the silicon nitride wafer customized in the step 1 is 65mm, the thickness of the silicon nitride wafer is 5mm, the length of the silicon nitride wedge is 65mm, and the cross section of the silicon nitride wedge is square with the side length of 2.4 mm.
According to the preparation method of the tantalum carbide chip, 2 silicon nitride wafers and 3 silicon nitride wedges are used in step 1.
According to the preparation method of the tantalum carbide sheet, the graphite powder wafer pressed in the step 2 is 65mm in diameter and 6mm in thickness.
According to the preparation method of the tantalum carbide sheet, in the step 3, the graphite heater comprises an upper cover and a cylinder body, the inner diameter of the cylinder body is 70mm, the outer diameter of the cylinder body is 90mm, the height of the cylinder body is 80mm, the depth of the cylinder body is 65mm, the outer diameter of the upper cover is 95mm, the inner diameter of the upper cover is 90mm, the height of the upper cover is 35mm, the depth of the upper cover is 20mm, and the upper cover is connected with the outer side of the upper end of the cylinder body through threads.
According to the preparation method of the tantalum carbide sheet, the centers of the silicon nitride wafer, the graphite powder wafer and the tantalum sheet are superposed in the step 4.
According to the preparation method of the tantalum carbide sheet, in the step 5, the protective gas is a mixed gas with the volume ratio of nitrogen to argon being 2: 1.
In the preparation method of the tantalum carbide sheet, in the step 6, absolute ethyl alcohol and acetone are respectively used for cleaning for 30min in an ultrasonic cleaning machine, and the ultrasonic frequency is 1000-10000 Hz.
According to the preparation method of the tantalum carbide sheet, the silicon nitride wafer and the silicon nitride wedge have the functions of isolating the graphite heater from being in contact with the graphite powder wafer, and preventing the whole conductor formed by the conduction between the graphite from interfering the normal work of the induction coil.
According to the preparation method of the tantalum carbide sheet, the graphite powder wafer is used for providing the carbon raw material and directly contacting with the tantalum sheet to perform a carbonization process; the space occupied by a large amount of graphite powder under the ordinary state is saved.
According to the preparation method of the tantalum carbide sheet, the centers of the circles of all the wafers are overlapped, and all the wafers cannot be attached to the inner wall of the heater under the fixation of the 3 wedges. The upper cover is screwed tightly. Because the total height of all the wafers is slightly higher than the inner depth of the heater, all the wafers are tightly pressed after the upper cover is screwed, and the wafers cannot move.
The preparation method of the tantalum carbide sheet can improve the flatness of the tantalum sheet after carbonization to the maximum extent.
The preparation method of the tantalum carbide sheet has the advantages of low cost, easy operation, convenient treatment and capability of being used at any time.
Drawings
FIG. 1 is a schematic view of the placement structure of silicon nitride wafers, graphite powder wafers and tantalum wafers in the graphite heater according to the present invention;
1 is a silicon nitride wafer, 2 is a graphite powder wafer, and 3 is a tantalum wafer.
Detailed Description
The first embodiment is as follows:
a preparation method of tantalum carbide sheets comprises the following steps:
step 4, charging, namely vertically placing silicon nitride wedges against the inner wall of a graphite heater, wherein the distance between every two silicon nitride wedges is equal, placing 1 silicon nitride wafer between 3 wedges, placing the silicon nitride wafers on the inner bottom surface of the graphite heater, placing 1 graphite powder wafer and 1 tantalum wafer on the silicon nitride wafers in sequence, then placing 1 graphite powder wafer and 1 tantalum wafer above the tantalum wafers, placing 6 graphite powder wafers and 5 tantalum wafers in sequence, then placing 1 silicon nitride wafer above the graphite powder wafers, and screwing the upper cover of the graphite heater;
step 5, putting the graphite heater installed in the step 4 into an induction heating furnace integrally, and vacuumizing to enable the vacuum degree to reach 10-4After Pa, raising the temperature to 1800 ℃ within 4 hours, then filling protective gas into the furnace to ensure that the furnace pressure reaches 750Torr, preserving the heat for 1 hour, then raising the furnace temperature to 2100 ℃, preserving the heat and maintaining the pressure for reaction for 20 hours, then cooling, and raising the furnace temperature to 1000 ℃ within 4 hours, and finishing the reaction;
and 6, opening the furnace to take out the graphite heater, taking out the tantalum sheet after reaction, and respectively cleaning the tantalum sheet by using absolute ethyl alcohol and acetone in an ultrasonic cleaning machine to obtain the tantalum carbide sheet.
In the method for preparing a tantalum carbide wafer according to the embodiment, the silicon nitride wafer customized in the step 1 has a diameter of 65mm and a thickness of 5mm, the silicon nitride wedge has a length of 65mm, and the cross section of the silicon nitride wedge is square with a side length of 2.4 mm.
In the method for preparing a tantalum carbide wafer according to the embodiment, in the step 1, 2 silicon nitride wafers and 3 silicon nitride wedges are used.
In the method for preparing tantalum carbide tablets in the embodiment, the graphite powder wafer pressed in the step 2 has a diameter of 65mm and a thickness of 6 mm.
In the preparation method of the tantalum carbide sheet in the embodiment, the graphite heater in the step 3 comprises an upper cover and a cylinder, the inner diameter of the cylinder is 70mm, the outer diameter of the cylinder is 90mm, the height of the cylinder is 80mm, the depth of the cylinder is 65mm, the outer diameter of the upper cover is 95mm, the inner diameter of the cylinder is 90mm, the height of the cylinder is 35mm, the depth of the cylinder is 20mm, and the outer sides of the upper ends of the upper cover and the cylinder are connected through threads.
In the method for preparing the tantalum carbide sheet according to the embodiment, the centers of the silicon nitride wafer, the graphite powder wafer and the tantalum sheet are superposed in step 4.
In the method for preparing a tantalum carbide sheet according to the embodiment, the protective gas in step 5 is a mixed gas of nitrogen and argon in a volume ratio of 2: 1.
In the preparation method of the tantalum carbide sheet according to the embodiment, in step 6, absolute ethyl alcohol and acetone are respectively used for cleaning for 30min in an ultrasonic cleaning machine, and the ultrasonic frequency is 2000 Hz.
In the method for preparing tantalum carbide sheet according to the embodiment, experimental data of the prepared tantalum carbide sheet are shown in fig. 1:
TABLE 1 Tantanium carbide sheet Properties
According to the method for preparing the tantalum carbide sheet, the prepared tantalum carbide sheet has high flatness.
In the preparation method of the tantalum carbide sheet, the silicon nitride wafer and the silicon nitride wedge have the functions of isolating the graphite heater from the graphite powder wafer, so that the whole conductor formed by the conduction between the graphite is prevented from interfering the normal work of the induction coil.
In the preparation method of the tantalum carbide sheet in the embodiment, the graphite powder wafer is used for providing the carbon raw material, and directly contacting with the tantalum sheet to perform the carbonization process; the space occupied by a large amount of graphite powder under the ordinary state is saved.
In the method for preparing the tantalum carbide sheet according to the embodiment, the centers of the circles of all the wafers are overlapped, and all the wafers cannot be attached to the inner wall of the heater under the fixation of the 3 wedges. The upper cover is screwed tightly. Because the total height of all the wafers is slightly higher than the inner depth of the heater, all the wafers are tightly pressed after the upper cover is screwed, and the wafers cannot move.
According to the preparation method of the tantalum carbide sheet, the flatness of the tantalum sheet after carbonization can be improved to the greatest extent.
The preparation method of the tantalum carbide sheet has the advantages of low cost, easy operation, convenient treatment and capability of being used at any time.
The second embodiment is as follows:
a preparation method of tantalum carbide sheets comprises the following steps:
step 4, charging, namely vertically placing silicon nitride wedges against the inner wall of a graphite heater, wherein the distance between every two silicon nitride wedges is equal, placing 1 silicon nitride wafer between 3 wedges, placing the silicon nitride wafers on the inner bottom surface of the graphite heater, placing 1 graphite powder wafer and 1 tantalum wafer on the silicon nitride wafers in sequence, then placing 1 graphite powder wafer and 1 tantalum wafer above the tantalum wafers, placing 6 graphite powder wafers and 5 tantalum wafers in sequence, then placing 1 silicon nitride wafer above the graphite powder wafers, and screwing the upper cover of the graphite heater;
step 5, putting the graphite heater installed in the step 4 into an induction heating furnace integrally, and vacuumizing to enable the vacuum degree to reach 10-4After Pa, raising the temperature to 1800 ℃ within 4 hours, then filling protective gas into the furnace to ensure that the furnace pressure reaches 750Torr, preserving the heat for 1 hour, then raising the furnace temperature to 2100 ℃, preserving the heat and maintaining the pressure for reaction for 20 hours, then cooling, and raising the furnace temperature to 1000 ℃ within 4 hours, and finishing the reaction;
and 6, opening the furnace to take out the graphite heater, taking out the tantalum sheet after reaction, and respectively cleaning the tantalum sheet by using absolute ethyl alcohol and acetone in an ultrasonic cleaning machine to obtain the tantalum carbide sheet.
According to the method for preparing the tantalum carbide sheet, the prepared tantalum carbide sheet has high flatness.
In the preparation method of the tantalum carbide sheet, the silicon nitride wafer and the silicon nitride wedge have the functions of isolating the graphite heater from the graphite powder wafer, so that the whole conductor formed by the conduction between the graphite is prevented from interfering the normal work of the induction coil.
In the preparation method of the tantalum carbide sheet in the embodiment, the graphite powder wafer is used for providing the carbon raw material, and directly contacting with the tantalum sheet to perform the carbonization process; the space occupied by a large amount of graphite powder under the ordinary state is saved.
In the method for preparing the tantalum carbide sheet according to the embodiment, the centers of the circles of all the wafers are overlapped, and all the wafers cannot be attached to the inner wall of the heater under the fixation of the 3 wedges. The upper cover is screwed tightly. Because the total height of all the wafers is slightly higher than the inner depth of the heater, all the wafers are tightly pressed after the upper cover is screwed, and the wafers cannot move.
According to the preparation method of the tantalum carbide sheet, the flatness of the tantalum sheet after carbonization can be improved to the greatest extent.
The preparation method of the tantalum carbide sheet has the advantages of low cost, easy operation, convenient treatment and capability of being used at any time.
The third concrete implementation mode:
according to the second specific embodiment, in the step 1, the diameter of the customized silicon nitride wafer is 65mm, the thickness of the customized silicon nitride wafer is 5mm, the length of the silicon nitride wedge is 65mm, and the cross section of the silicon nitride wedge is a square with the side length of 2.4 mm.
The fourth concrete implementation mode:
according to the second specific embodiment, in the step 1, 2 silicon nitride wafers and 3 silicon nitride wedges are used.
The fifth concrete implementation mode:
according to the second specific embodiment of the method for preparing tantalum carbide tablets, the graphite powder wafer pressed in the step 2 has a diameter of 65mm and a thickness of 6 mm.
The sixth specific implementation mode:
according to the second specific embodiment, in the step 3, the graphite heater comprises an upper cover and a cylinder, the inner diameter of the cylinder is 70mm, the outer diameter of the cylinder is 90mm, the height of the cylinder is 80mm, the depth of the cylinder is 65mm, the outer diameter of the upper cover is 95mm, the inner diameter of the cylinder is 90mm, the height of the cylinder is 35mm, the depth of the cylinder is 20mm, and the upper cover is connected with the outer side of the upper end of the cylinder through threads.
The seventh embodiment:
according to the second specific embodiment, in the step 4, the centers of the silicon nitride wafer, the graphite powder wafer and the tantalum sheet are superposed.
The specific implementation mode is eight:
according to the second specific embodiment of the method for preparing tantalum carbide sheet, in the step 5, the protective gas is a mixed gas of nitrogen and argon in a volume ratio of 2: 1.
The specific implementation method nine:
according to the second specific embodiment, in step 6, the tantalum carbide sheet is cleaned with absolute ethyl alcohol and acetone in an ultrasonic cleaner for 30min, wherein the ultrasonic frequency is 1000-10000 Hz.
Claims (8)
1. A preparation method of tantalum carbide sheets is characterized by comprising the following steps: the method comprises the following steps:
step 1, customizing a silicon nitride wafer and a silicon nitride wedge;
step 2, pressing the graphite powder wafer by using a hydraulic press;
step 3, customizing a graphite heater;
step 4, charging, namely vertically placing silicon nitride wedges against the inner wall of a graphite heater, wherein the distance between every two silicon nitride wedges is equal, placing 1 silicon nitride wafer between 3 wedges, placing the silicon nitride wafers on the inner bottom surface of the graphite heater, placing 1 graphite powder wafer and 1 tantalum wafer on the silicon nitride wafers in sequence, then placing 1 graphite powder wafer and 1 tantalum wafer above the tantalum wafers, placing 6 graphite powder wafers and 5 tantalum wafers in sequence, then placing 1 silicon nitride wafer above the graphite powder wafers, and screwing the upper cover of the graphite heater;
step 5, putting the graphite heater installed in the step 4 into an induction heating furnace integrally, and vacuumizing to enable the vacuum degree to reach 10-4After Pa, raising the temperature to 1800 ℃ within 4 hours, then filling protective gas into the furnace to ensure that the furnace pressure reaches 750Torr, preserving the heat for 1 hour, then raising the furnace temperature to 2100 ℃, preserving the heat and maintaining the pressure for reaction for 20 hours, then cooling, and raising the furnace temperature to 1000 ℃ within 4 hours, and finishing the reaction;
and 6, opening the furnace to take out the graphite heater, taking out the tantalum sheet after reaction, and respectively cleaning the tantalum sheet by using absolute ethyl alcohol and acetone in an ultrasonic cleaning machine to obtain the tantalum carbide sheet.
2. The method for preparing tantalum carbide sheet according to claim 1, wherein: the diameter of the silicon nitride wafer customized in the step 1 is 65mm, the thickness of the silicon nitride wafer is 5mm, the length of the silicon nitride wedge is 65mm, and the cross section of the silicon nitride wedge is a square with the side length of 2.4 mm.
3. The method for producing tantalum carbide sheet according to claim 1 or 2, wherein: in the step 1, 2 silicon nitride wafers and 3 silicon nitride wedges are used.
4. The method for preparing tantalum carbide sheet according to claim 3, wherein: the graphite powder wafer pressed in the step 2 has a diameter of 65mm and a thickness of 6 mm.
5. The method for preparing tantalum carbide sheet according to claim 4, wherein: the graphite heater in the step 3 comprises an upper cover and a cylinder body, wherein the inner diameter of the cylinder body is 70mm, the outer diameter of the cylinder body is 90mm, the height of the cylinder body is 80mm, the depth of the cylinder body is 65mm, the outer diameter of the upper cover is 95mm, the inner diameter of the upper cover is 90mm, the height of the upper cover is 35mm, the depth of the upper cover is 20mm, and the outer sides of the upper ends of the upper cover and the cylinder body are connected through threads.
6. The method for preparing tantalum carbide sheet according to claim 5, wherein: in the step 4, the centers of the silicon nitride wafer, the graphite powder wafer and the tantalum wafer are superposed.
7. The method for preparing tantalum carbide sheet according to claim 6, wherein: and in the step 5, the protective gas is a mixed gas of nitrogen and argon in a volume ratio of 2: 1.
8. The method for preparing tantalum carbide sheet according to claim 7, wherein: and 6, respectively cleaning the glass substrate with absolute ethyl alcohol and acetone for 30min in an ultrasonic cleaning machine, wherein the ultrasonic frequency is 1000-.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115874279A (en) * | 2023-02-28 | 2023-03-31 | 中国电子科技集团公司第四十六研究所 | Preparation method of tantalum carbide substrate for growing aluminum nitride on silicon carbide |
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