CN113387337A - Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method - Google Patents
Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method Download PDFInfo
- Publication number
- CN113387337A CN113387337A CN202110569857.5A CN202110569857A CN113387337A CN 113387337 A CN113387337 A CN 113387337A CN 202110569857 A CN202110569857 A CN 202110569857A CN 113387337 A CN113387337 A CN 113387337A
- Authority
- CN
- China
- Prior art keywords
- furnace body
- titanium
- powder
- shell
- titanium powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000005121 nitriding Methods 0.000 title claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 78
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000005485 electric heating Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 53
- 229910052750 molybdenum Inorganic materials 0.000 claims description 53
- 239000011733 molybdenum Substances 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 19
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
- C01B21/0761—Preparation by direct nitridation of titanium, zirconium or hafnium
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/02—Ohmic resistance heating
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
- F27D2007/066—Vacuum
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
- F27D2009/0002—Cooling of furnaces
- F27D2009/001—Cooling of furnaces the cooling medium being a fluid other than a gas
- F27D2009/0013—Cooling of furnaces the cooling medium being a fluid other than a gas the fluid being water
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
- F27D2009/0002—Cooling of furnaces
- F27D2009/0018—Cooling of furnaces the cooling medium passing through a pattern of tubes
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The equipment for preparing the titanium nitride powder by the titanium powder direct nitriding method is optimized, the titanium powder uniformly spread on the equipment is heated by the electric heating device, and the heating uniformity of the titanium powder is improved, so that the full reaction of nitrogen with constant concentration in a furnace body and the titanium powder is facilitated, the nitrogen content of the titanium nitride powder is improved, the preparation quality of the titanium nitride powder is ensured, the preparation process is simple, the synthesis effect is good, the preparation cost is low, and the preparation efficiency is high.
Description
Technical Field
The invention belongs to the technical field of titanium nitride powder preparation, and particularly relates to equipment for preparing high titanium nitride powder by a titanium powder nitriding method and a process method thereof.
Background
Titanium nitride is a novel material, has the characteristics of high hardness (microhardness of 21GPa), high melting point (2950 ℃) and good chemical stability, and is a good refractory and wear-resistant material. The titanium nitride also has good conductivity, and can be used as conductive materials of electrodes, electrical contacts and the like for molten salt electrolysis and superconducting materials with higher superconducting critical temperature. In addition, it has good biocompatibility and can be used as biological material. At present, there are many methods for preparing titanium nitride, including (1) direct nitridation of metallic titanium powder, (2) microwave carbothermic reduction, (3) reductive nitridation of titanium oxide, (4) self-propagating high-temperature synthesis, (5) solvothermal synthesis, (6) mechanical alloying, (7) sol-gel process, (8) chemical vapor deposition; the existing equipment and process for preparing titanium nitride powder by using a direct nitridation method of metal titanium powder have the problems that the titanium powder cannot fully react with nitrogen, so that the color, the hardness and the like of the produced titanium nitride cannot meet the requirements, the loss is large, and the preparation cost is high, so that improvement is needed for solving the problems.
Disclosure of Invention
The technical problems solved by the invention are as follows: the equipment for preparing the titanium nitride powder by the titanium powder direct nitriding method is optimized, the titanium powder uniformly spread on the equipment is heated by the electric heating device, and the heating uniformity of the titanium powder is improved, so that the full reaction of nitrogen with constant concentration in a furnace body and the titanium powder is facilitated, the nitrogen content of the titanium nitride powder is improved, the preparation quality of the titanium nitride powder is ensured, the preparation process is simple, the synthesis effect is good, the preparation cost is low, and the preparation efficiency is high.
The technical scheme adopted by the invention is as follows: the equipment for preparing the high-titanium nitride powder by the titanium powder nitriding method comprises a shell and a furnace body, wherein an upper furnace mouth is arranged in the shell and extends out of the furnace body which is arranged on the shell, a water cooling circulation system is arranged between the furnace body and the shell, the upper end of the shell is detachably fixed with an upper cover which is used for sealing the furnace mouth on the furnace body, an electric heating device and titanium powder are arranged in the furnace body and are arranged on a heating surface of the electric heating device, the electric heating device is electrically connected with a frequency conversion cabinet outside the equipment through a wire, the upper end side wall of the shell is provided with an inner end and a vacuumizing joint which is communicated with the inside of the furnace body, and the outer end of the inner end of the vacuumizing joint passes through a pipeline and is connected with a vacuum pump, and the upper cover is provided with an observation window and a safety valve, a vacuum pressure gauge and a nitrogen adding pipe which are arranged outside the observation window.
The electric heating device comprises a molybdenum plate and mounting seats, the mounting seats are arranged on two sides of the lower end in the furnace body, two ends of the molybdenum plate are respectively arranged on the mounting seats on the corresponding sides, positive electrodes and negative electrodes are arranged on two side walls of the shell in an insulating mode, the inner end portions of the positive electrodes and the negative electrodes penetrate through the furnace body and are connected with the side walls of the upper ends of the mounting seats on the corresponding sides, the outer end portions of the positive electrodes and the negative electrodes extend out of the shell, and the positive electrodes and the negative electrodes are electrically connected with the frequency conversion cabinet through wires.
Furthermore, the side walls of the two ends of the molybdenum plate are of a tapered structure with a large upper part and a small lower part, the mounting seat is composed of a support column and a support seat which is fixed at the upper end of the support column and supported by a conductive material, the cross section of the support seat is of an L-shaped structure, the inner edge of the support seat is of a tapered structure matched with the end part of the molybdenum plate, the inner end parts of the positive electrode and the negative electrode are in contact with the outer wall of the corresponding side support seat, and the two ends of the molybdenum plate are clamped on the support seat on the corresponding side.
Further, water-cooling circulation system is including locating the water circulation coil pipe in the interlayer between furnace body and the casing, water circulation coil pipe lower extreme and the inlet tube intercommunication that is fixed in on the outer wall of casing lower extreme, water circulation coil pipe upper end and the outlet pipe intercommunication of locating on the outer wall of casing upper end.
Furthermore, a water cooling circulation system is also arranged on the upper cover.
Furthermore, the observation window is made of high-temperature-resistant glass, the upper cover is matched with the furnace opening at the upper end of the furnace body, a sealing ring is arranged between the upper cover and the furnace opening at the upper end of the furnace body, and the upper cover is detachably fixed at the upper end of the shell through a plurality of lock catches.
The process method for preparing the high titanium nitride powder by the titanium powder nitriding method comprises the following steps:
1) installing a molybdenum plate: opening the upper cover, and arranging the molybdenum plates on the two supporting seats to enable the side walls of the molybdenum plates to be tightly attached to the inner walls of the supporting seats after being matched;
2) loading titanium powder: after the molybdenum plate is reliably and stably installed, titanium powder is flatly arranged on the molybdenum plate, so that the titanium powder is uniformly heated after the molybdenum plate is electrified and heated, then the upper cover is covered, and the upper cover is fixed at the upper end of the shell through a plurality of lock catches, so that a furnace mouth at the upper end of the furnace body is reliably sealed;
3) tank washing: vacuumizing the furnace body through a vacuum pump connected with a vacuumizing joint, adding nitrogen into the furnace body through a nitrogen adding pipe, and finishing the removal of impurity gas in the furnace body after repeating the vacuumizing and nitrogen adding processes for multiple times;
4) reaction: and adding nitrogen into the furnace body after the tank is washed to 0.08-0.12 Pa, electrically connecting a low-voltage high-current power supply processed by the frequency conversion cabinet with the positive electrode and the negative electrode and supplying power to the molybdenum plate, heating the titanium powder on the molybdenum plate at high temperature by the molybdenum plate, reacting the titanium powder with the nitrogen in the furnace body to generate high-purity titanium nitride powder, and continuously adding the nitrogen into the furnace body in the reaction process to keep the internal pressure constant.
In the step 3), the furnace body is subjected to two repeated processes of vacuumizing and adding nitrogen, so that the impurity gas in the furnace body can be removed, the furnace body is pumped by a vacuum pump to a vacuum pressure gauge to display that the pressure in the furnace body is-0.08 to-0.12 Pa and then stops, the furnace body is added with nitrogen to the vacuum pressure gauge to display that the pressure in the furnace body is 0.08 to 0.12Pa and then stops, and the safety valve starts to release gas when the pressure value in the furnace body is more than 0.2 Pa.
In the step 4), the high current range of the low-voltage high-current power supply processed by the frequency conversion cabinet is 1600-2000A, and the low voltage range is 45-55V.
Compared with the prior art, the invention has the advantages that:
1. according to the technical scheme, the equipment for preparing the titanium nitride powder by the direct titanium powder nitriding method is optimized, the electric heating device is adopted to heat the titanium powder uniformly spread on the equipment, and the heating uniformity of the titanium powder is improved, so that the full reaction of nitrogen with constant concentration in a furnace body and the titanium powder is facilitated, and the nitrogen content of the titanium nitride powder is improved;
2. according to the technical scheme, the supporting seat with the inner wall of a conical structure with the large upper part and the small lower part is adopted to be matched with the molybdenum plate, so that on one hand, the stability of the molybdenum plate after the molybdenum plate is installed on the supporting seat can be ensured, on the other hand, the good contact between the inner side wall of the supporting seat and the side wall of the molybdenum plate is facilitated, and the reliable and effective transmission of current to the molybdenum plate is ensured;
3. according to the technical scheme, impurity gases in the furnace body are removed in a mode that the processes of vacuumizing and adding nitrogen are repeated for multiple times, so that the influence of other impurity gases in the furnace body in the reaction process of titanium powder and nitrogen is effectively avoided, and the quality of titanium nitride is improved;
4. the technical scheme has the advantages of simple preparation process, good synthesis effect, low preparation cost and high preparation efficiency, ensures the preparation quality of the titanium nitride powder, and ensures high hardness of the prepared titanium nitride.
Drawings
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a top view of the upper cover of the present invention.
Detailed Description
In the following, an embodiment of the present invention will be described in conjunction with fig. 1-2, so as to clearly and completely describe the technical solutions, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, but not all of the embodiment.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
The equipment for preparing the high titanium nitride powder by the titanium powder nitriding method comprises a shell 1 and a furnace body 2, wherein a furnace body 2 with an upper furnace mouth extending out of the shell 1 is arranged in the shell 1, a water cooling circulating system is arranged between the furnace body 2 and the shell 1, an upper cover 4 used for sealing the furnace mouth at the upper end of the furnace body 2 is detachably fixed at the upper end of the shell 1, an electric heating device is arranged in the furnace body 2 and the titanium powder is arranged on a heating surface of the electric heating device, the electric heating device is electrically connected with a frequency conversion cabinet at the outer side of the equipment through a lead, a vacuumizing joint 5 with an inner end communicated with the inside of the furnace body 2 and an outer end connected with a vacuum pump through a pipeline is arranged on the side wall at the upper end of the shell 1, and an observation window 6, a safety valve 7 positioned outside the observation window 6, a vacuum pressure gauge 8 and a nitrogen adding pipe 3 are arranged on the upper cover 4; in the structure, the equipment for preparing the titanium nitride powder by the direct titanium powder nitriding method is optimized, and the electric heating device is adopted to heat the titanium powder uniformly spread on the equipment, so that the heating uniformity of the titanium powder is improved, the full reaction of nitrogen with constant concentration in the furnace body 2 and the titanium powder is facilitated, and the nitrogen content of the titanium nitride powder is improved;
the specific structure of the electric heating device is as follows: the electric heating device comprises a molybdenum plate 9 and mounting seats 10, the mounting seats 10 are respectively arranged on two sides of the lower end in the furnace body 2, two ends of the molybdenum plate 9 are respectively arranged on the mounting seats 10 on the corresponding side, the two side walls of the shell 1 are provided with an anode 11 and a cathode 12 in an insulating way, the inner end parts of the anode 11 and the cathode 12 penetrate through the furnace body 2 and are connected with the upper end side wall of the mounting seat 10 on the corresponding side, the outer end parts of the anode 11 and the cathode 12 extend out of the shell 1, and the anode 11 and the cathode 12 are electrically connected with the frequency conversion cabinet through wires; specifically, the side walls of two ends of the molybdenum plate 9 are in a tapered structure with a large top and a small bottom, the mounting seat 10 is composed of a support pillar 10-1 and a support seat 10-2 which is fixed at the upper end of the support pillar 10-1 and supported by a conductive material, the cross section of the support seat 10-2 is in an L-shaped structure, the inner edge of the support seat 10-2 is in a tapered structure matched with the end of the molybdenum plate 9, the inner ends of the positive electrode 11 and the negative electrode 12 are in contact with the outer wall of the support seat 10-2 corresponding to the side, and two ends of the molybdenum plate 9 are clamped on the support seat 10-2 corresponding to the; the structure of the electric heating device provides a heating condition for the reaction of the titanium powder and the nitrogen, and ensures the uniformity of the heating of the titanium powder flattened on the molybdenum plate 9.
The water cooling circulation system has the following specific structure: the water cooling circulation system comprises a water circulation coil pipe arranged in an interlayer between the furnace body 2 and the shell 1, the lower end of the water circulation coil pipe is communicated with a water inlet pipe 14 fixed on the outer wall of the lower end of the shell 1, and the upper end of the water circulation coil pipe is communicated with a water outlet pipe 13 arranged on the outer wall of the upper end of the shell 1, so that potential safety hazards caused by overheating of the shell 1 are avoided; specifically, also be equipped with water cooling circulation system on the upper cover 4, can avoid the overheated potential safety hazard that causes of upper cover 4 on the one hand, on the other hand can reduce the influence of temperature to the sealing washer, slows down ageing speed, improves the life of sealing washer.
The observation window 6 is made of high-temperature-resistant glass, the upper cover 4 is matched with the upper end furnace opening of the furnace body 2, a sealing ring is arranged between the upper cover 4 and the upper end furnace opening of the furnace body 2, and the upper cover 4 is detachably fixed at the upper end of the shell 1 through a plurality of lock catches.
The process method for preparing the high titanium nitride powder by the titanium powder nitriding method comprises the following steps:
1) installing a molybdenum plate 9: opening the upper cover 4, and installing the molybdenum plate 9 on the two supporting seats 10-2 to ensure that the side wall of the molybdenum plate 9 is tightly attached to the inner walls of the supporting seats 10-2 after being matched; the supporting connection structure which is matched with the molybdenum plate and provided with the supporting seat 10-2 with the inner wall of a conical structure with a large upper part and a small lower part is adopted, so that the stability of the molybdenum plate after the molybdenum plate is installed on the supporting seat 10-2 can be ensured, the good contact between the inner side wall of the supporting seat 10-2 and the side wall of the molybdenum plate 9 is facilitated, and the reliable and effective transmission of current to the molybdenum plate 9 is ensured;
2) loading titanium powder: after the molybdenum plate 9 is reliably and stably installed, titanium powder is flatly arranged on the molybdenum plate 9, so that the titanium powder is uniformly heated after the molybdenum plate 9 is electrified and heated, then the upper cover 4 is covered, and the upper cover 4 is fixed at the upper end of the shell 1 through a plurality of lock catches, so that a furnace mouth at the upper end of the furnace body 2 is reliably sealed; 3) tank washing: vacuumizing the furnace body 2 by a vacuum pump connected with a vacuumizing joint 5, adding nitrogen into the furnace body 1 by a nitrogen adding pipe 3, and finishing the removal of impurity gas in the furnace body 2 after repeating the vacuumizing and nitrogen adding processes for a plurality of times; specifically, after the two processes of vacuumizing and adding nitrogen are repeated twice, the impurity gas in the furnace body 2 can be removed, the furnace body 2 is vacuumized by a vacuum pump to a vacuum pressure gauge 8 to display that the pressure in the furnace body 2 reaches-01 Pa and then stops, the furnace body 2 is added with nitrogen to the vacuum pressure gauge 8 to display that the pressure in the furnace body 2 reaches 0.1Pa and then stops, and when the pressure value in the furnace body 2 is more than 0.2Pa, a safety valve 7 is started to release gas, so that the safety and reliability of the titanium nitride preparation process are improved; the impurity gas in the furnace body 2 is removed by repeating the vacuum-pumping and nitrogen-adding processes for a plurality of times, so that the influence of other impurity gases in the furnace body 2 in the reaction process of titanium powder and nitrogen is effectively avoided, and the quality of titanium nitride is improved;
4) reaction: adding nitrogen into the furnace body 2 after tank washing to 0.1Pa, electrically connecting a low-voltage high-current power supply processed by a frequency conversion cabinet with a positive electrode 11 and a negative electrode 12, supplying power to a molybdenum plate 9, heating titanium powder on the molybdenum plate 9 at high temperature, reacting the titanium powder with the nitrogen in the furnace body 2 to generate high-purity titanium nitride powder, and continuously adding the nitrogen into the furnace body 2 in the reaction process to keep the internal pressure constant; specifically, in step 4, the high current range of the low-voltage high-current power supply processed by the frequency conversion cabinet is 1800A, the low voltage range is 50V, and the safety is high.
The technical scheme has the advantages of simple preparation process, good synthesis effect, low preparation cost and high preparation efficiency, ensures the preparation quality of the titanium nitride powder, and ensures the hardness of the prepared titanium nitride.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and therefore, all equivalent changes made by the contents of the claims of the present invention should be included in the claims of the present invention.
Claims (9)
1. The equipment for preparing the high titanium nitride powder by the titanium powder nitriding method is characterized in that: comprises a shell (1) and a furnace body (2), the furnace body (2) with an upper furnace mouth extending out of the shell (1) is arranged in the shell (1), a water cooling circulation system is arranged between the furnace body (2) and the shell (1), an upper cover (4) used for sealing a furnace mouth at the upper end of the furnace body (2) is detachably fixed at the upper end of the shell (1), an electric heating device is arranged in the furnace body (2) and the titanium powder is arranged on the heating surface of the electric heating device, the electric heating device is electrically connected with a frequency conversion cabinet outside the equipment through a lead, the side wall of the upper end of the shell (1) is provided with a vacuumizing joint (5) of which the inner end is communicated with the inside of the furnace body (2) and the outer end is connected with a vacuum pump through a pipeline, and the upper cover (4) is provided with an observation window (6), a safety valve (7) positioned on the outer side of the observation window (6), a vacuum pressure gauge (8) and a nitrogen adding pipe (3).
2. The apparatus for preparing titanium powder with high titanium nitride by titanium powder nitriding method according to claim 1, characterized in that: the electric heating device comprises a molybdenum plate (9) and a mounting seat (10), the mounting seats (10) are arranged on two sides of the lower end in the furnace body (2), two ends of the molybdenum plate (9) are respectively arranged on the mounting seats (10) on the corresponding sides, the inner end parts of the two side walls of the shell (1) are installed on the side walls of the corresponding side in an insulating mode, penetrate through the furnace body (2) and are connected with the side wall of the upper end of the mounting seat (10) on the corresponding side, the outer end parts of the two side walls of the shell (1) extend out of a positive electrode (11) and a negative electrode (12) arranged on the shell (1), and the positive electrode (11) and the negative electrode (12) are electrically connected with the frequency conversion cabinet through wires.
3. The apparatus for preparing titanium powder with high titanium nitride by titanium powder nitriding method according to claim 2, characterized in that: the molybdenum plate comprises a molybdenum plate (9), wherein the side walls of two ends of the molybdenum plate (9) are of a tapered structure with a large upper part and a small lower part, the mounting seat (10) is composed of a supporting column (10-1) and a supporting seat (10-2) which is fixed at the upper end of the supporting column (10-1) and is supported by a conductive material, the cross section of the supporting seat (10-2) is of an L-shaped structure, the inner edge of the supporting seat (10-2) is of a tapered structure matched with the end part of the molybdenum plate (9), the inner end parts of the positive electrode (11) and the negative electrode (12) are in contact with the outer wall of the corresponding side supporting seat (10-2), and two ends of the molybdenum plate (9) are clamped on the supporting seat (10-2) of the corresponding side.
4. The apparatus for preparing titanium powder with high titanium nitride by titanium powder nitriding method according to claim 1, characterized in that: the water-cooling circulation system comprises a water circulation coil pipe arranged between the furnace body (2) and the shell (1) and arranged in a sandwich layer, the lower end of the water circulation coil pipe is communicated with a water inlet pipe (14) fixed on the outer wall of the lower end of the shell (1), and the upper end of the water circulation coil pipe is communicated with a water outlet pipe (13) arranged on the outer wall of the upper end of the shell (1).
5. The apparatus for preparing titanium powder with high titanium nitride according to claim 4, wherein: and a water cooling circulation system is also arranged on the upper cover (4).
6. The apparatus for preparing titanium powder with high titanium nitride by titanium powder nitriding method according to claim 1, characterized in that: the observation window (6) is made of high-temperature-resistant glass, the upper cover (4) is matched with the upper end furnace opening of the furnace body (2), a sealing ring is arranged between the upper cover (4) and the upper end furnace opening of the furnace body (2), and the upper cover (4) is detachably fixed on the upper end of the shell (1) through a plurality of lock catches.
7. The process method for preparing the high titanium nitride powder by the titanium powder nitriding method is characterized by comprising the following steps:
1) mounting a molybdenum plate (9): opening the upper cover (4), and arranging the molybdenum plate (9) on the two supporting seats (10-2) to ensure that the side wall of the molybdenum plate (9) is tightly attached after being matched with the inner walls of the supporting seats (10-2);
2) loading titanium powder: after the molybdenum plate (9) is reliably and stably installed, titanium powder is flatly arranged on the molybdenum plate (9), so that the titanium powder is uniformly heated after the molybdenum plate (9) is electrified and heated, then the upper cover (4) is covered, and the upper cover (4) is fixed at the upper end of the shell (1) through a plurality of lock catches, so that a furnace mouth at the upper end of the furnace body (2) is reliably sealed;
3) tank washing: vacuumizing the furnace body (2) through a vacuum pump connected with a vacuumizing joint (5), adding nitrogen into the furnace body (1) through a nitrogen adding pipe (3), and finishing the removal of impurity gas in the furnace body (2) after repeating the vacuumizing and nitrogen adding processes for multiple times;
4) reaction: and adding nitrogen into the furnace body (2) after the tank is washed to 0.08-0.12 Pa, electrically connecting a low-voltage high-current power supply processed by the frequency conversion cabinet with the positive electrode (11) and the negative electrode (12), supplying power to the molybdenum plate (9), heating the titanium powder on the molybdenum plate at high temperature, reacting the titanium powder with the nitrogen in the furnace body (2) to generate high-purity titanium nitride powder, and continuously adding the nitrogen into the furnace body (2) in the reaction process to keep the internal pressure constant.
8. The process method for preparing high titanium nitride powder by the titanium powder nitriding method according to claim 7, characterized in that: in the step 3), the furnace body (2) is vacuumized and nitrogen-added twice, and then the impurity gas in the furnace body (2) can be removed, the furnace body (2) is vacuumized by a vacuum pump until a vacuum pressure gauge (8) displays that the pressure in the furnace body (2) is between-0.08 and-0.12 Pa, and then the furnace body is stopped, the furnace body (2) is added with nitrogen until a vacuum pressure gauge (8) displays that the pressure in the furnace body (2) is between 0.08 and 0.12Pa, and then the furnace body (2) is stopped, and when the pressure value in the furnace body (2) is greater than 0.2Pa, a safety valve (7) is started to release gas.
9. The process method for preparing high titanium nitride powder by titanium powder nitriding according to claim 8, characterized in that: in the step 4), the high current range of the low-voltage high-current power supply processed by the frequency conversion cabinet is 1600-2000A, and the low voltage range is 45-55V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110569857.5A CN113387337A (en) | 2021-05-25 | 2021-05-25 | Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110569857.5A CN113387337A (en) | 2021-05-25 | 2021-05-25 | Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113387337A true CN113387337A (en) | 2021-09-14 |
Family
ID=77618952
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110569857.5A Pending CN113387337A (en) | 2021-05-25 | 2021-05-25 | Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113387337A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1010651A (en) * | 1960-11-03 | 1965-11-24 | Ti Group Services Ltd | Manufacture of metal nitrides |
| CN1603238A (en) * | 2004-09-27 | 2005-04-06 | 南京大学 | Preparation method of titanium carbide and titanium nitride one dimension nanometer construction material |
| WO2017170857A1 (en) * | 2016-03-30 | 2017-10-05 | 新日鉄住金マテリアルズ株式会社 | Device for manufacturing spherical aluminum nitride particles |
| CN109437132A (en) * | 2018-12-14 | 2019-03-08 | 中信锦州金属股份有限公司 | A kind of production method nitrogenizing titanium valve |
| CN208747636U (en) * | 2018-02-24 | 2019-04-16 | 吉林长玉特陶新材料技术股份有限公司 | A kind of quick production titanium carbonitride, the device for nitrogenizing powder |
| CN209085329U (en) * | 2018-08-13 | 2019-07-09 | 信阳市德隆超硬材料有限公司 | Nitriding furnace cooling device |
| CN209442649U (en) * | 2018-12-25 | 2019-09-27 | 洛阳彤润信息科技有限公司 | A kind of nanoscale nitridation titanium valve preparation facilities |
-
2021
- 2021-05-25 CN CN202110569857.5A patent/CN113387337A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1010651A (en) * | 1960-11-03 | 1965-11-24 | Ti Group Services Ltd | Manufacture of metal nitrides |
| CN1603238A (en) * | 2004-09-27 | 2005-04-06 | 南京大学 | Preparation method of titanium carbide and titanium nitride one dimension nanometer construction material |
| WO2017170857A1 (en) * | 2016-03-30 | 2017-10-05 | 新日鉄住金マテリアルズ株式会社 | Device for manufacturing spherical aluminum nitride particles |
| CN208747636U (en) * | 2018-02-24 | 2019-04-16 | 吉林长玉特陶新材料技术股份有限公司 | A kind of quick production titanium carbonitride, the device for nitrogenizing powder |
| CN209085329U (en) * | 2018-08-13 | 2019-07-09 | 信阳市德隆超硬材料有限公司 | Nitriding furnace cooling device |
| CN109437132A (en) * | 2018-12-14 | 2019-03-08 | 中信锦州金属股份有限公司 | A kind of production method nitrogenizing titanium valve |
| CN209442649U (en) * | 2018-12-25 | 2019-09-27 | 洛阳彤润信息科技有限公司 | A kind of nanoscale nitridation titanium valve preparation facilities |
Non-Patent Citations (1)
| Title |
|---|
| 谈国强等: "合成氧化钛粉体的研究进展", 《陕西科技大学学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20100147219A1 (en) | High temperature and high voltage electrode assembly design | |
| US2760930A (en) | Electrolytic cell of the diaphragm type | |
| TWI495029B (en) | Manufacturing apparatus for depositing a material and an electrode for use therein | |
| CN103270198B (en) | Electrolysis installation | |
| CN103237926A (en) | Method and system for electrolytically reducing a solid feedstock | |
| JP7428411B2 (en) | Systems and methods for molten oxide electrolysis | |
| CN203474925U (en) | High temperature continuous electrolysis experimental furnace with good sealing structure | |
| JP6461329B2 (en) | Silicon oxide manufacturing apparatus and preparation method | |
| CN113387337A (en) | Equipment and process method for preparing high-titanium-nitride powder by titanium powder nitriding method | |
| CN105202908A (en) | Vacuum consumable electrode arc furnace | |
| CN108360025B (en) | A kind of method that aqueous solution electrolysis solid metallic sulfide prepares metal | |
| CN110220376A (en) | A kind of Electric Arc smelting furnace | |
| CN105908031B (en) | Aluminum alloy materials of high conductivity and preparation method thereof | |
| CN214218825U (en) | Device for preparing metal vanadium by microwave heating | |
| CN100543176C (en) | The magnetron sputtering cathode target that is used for ultra-high vacuum system | |
| CN217103087U (en) | Reaction furnace for graphite purification | |
| KR101133151B1 (en) | Method for manufacturing electrode for vapor deposition process | |
| CN2516568Y (en) | Chlorine trifluoride electric tank | |
| CN104928721A (en) | Preparation and refining device for low-valent titanium chloride molten salt electrolyte | |
| CN115076596A (en) | Water electrolysis hydrogen production and hydrogenation integrated hydrogenation station system and process | |
| CN113755907A (en) | Baker device for fused salt rare earth electrolysis cell | |
| CN202543039U (en) | Automatic sealing-off furnace for vacuum device by means of electromagnetic induction heating fusion | |
| CN216864352U (en) | Electrolysis device | |
| CN212865011U (en) | Electrolytic cell for tungsten hexafluoride processing | |
| CN208145495U (en) | A kind of two-stage vacuum device for protecting reactor tank |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210914 |