CN103253675A - Preparation method of superfine ZrSi powder - Google Patents
Preparation method of superfine ZrSi powder Download PDFInfo
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- CN103253675A CN103253675A CN2013102351987A CN201310235198A CN103253675A CN 103253675 A CN103253675 A CN 103253675A CN 2013102351987 A CN2013102351987 A CN 2013102351987A CN 201310235198 A CN201310235198 A CN 201310235198A CN 103253675 A CN103253675 A CN 103253675A
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Abstract
The invention relates to a preparation method of superfine ZrSi powder, which comprises the steps that (1) batching is conducted by the following materials according to a mass percentage: 84.36-108.46 of Mg, 216.31-278.12 of ZrO2, 49.31-63.40 of Si and 50.00-150.00 of NaCl; (2) ball milling is conducted; (3) reaction materials are placed in a mold after uniformly mixed, and pressed into a cake-shaped blank; a tablet ignition agent is put in a copper crucible in a reaction kettle; the pressed blank is placed on the ignition agent; (4) the reaction kettle is sealed; argon is filled in the reaction kettle at a room temperature, exhausted when the temperature is raised to 120 DEG C, exhausted again when the temperature in the reaction kettle is raised to 180-200 DEG C, and filled again when the reading of a pressure gauge is reduced to zero; (5) when the temperature in the reaction kettle reaches 250-295 DEG C, the ignition agent is burnt; a reaction is self-maintained under the condition of self heat release; a block material containing a ZrSi product is obtained; (6) the block material containing the ZrSi product is cooled to the room temperature with the reaction kettle, ground into the power, and subjected to leaching treatment with hydrochloric acid; and (7) leached ZrSi is separated from leaching liquor, washed, and dried.
Description
Technical field
The present invention relates to the technology of preparing of ZrSi powder body material.
Background technology
ZrSi also is a kind of important metal silicide materials, has special physical properties and chemical property.ZrSi has high melt point, and this makes it become a kind of well behaved refractory materials; ZrSi has high density and uniform structure, can be used to make a kind of high barrier material; Can prepare a kind of new structured material that has good prospects with ZrSi, have high specific conductivity and thermal conductivity in this kind novel material corrosive medium at high temperature.The ZrSi antioxidant property is good, and at high temperature the surface oxidation of ZrSi generates ZrO
2, SiO
2And ZrSiO
4Oxide compound, ZrO
2, SiO
2And ZrSiO
4Oxide compound form a kind of zone of oxidation on its surface, just prevented the further oxidation on its surface just because of the existence of this zone of oxidation, this makes it at high temperature have good antioxidant property.The energy consumption of prior art is bigger, and cost is higher.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of ultra-fine ZrSi powder.
The present invention isA kind of preparation method of ultra-fine ZrSi powder the steps include:
(1) by mass percentage, according to Mg:84.36～108.46, ZrO
2: 216.31～278.12, prepare burden in Si:49.31～63.40, NaCl:50.00～150.00;
(2) the good raw material of weighing carries out ball milling, and time remaining 8～12h evenly mixes its powder;
(3) reaction mass mixes and is placed in the mould, and pressure-controlling is pressed into reaction mass the round pie blank under 10～20MPa; In reactor, put the tablet detonator in the copper crucible, again the blank that suppresses is placed on the detonator;
(4) sealed reactor at room temperature charges into 0.5～1.5MPa argon gas in reactor, open reactor heating trip switch then, is warming up to 120 ℃ of exhausts, to get rid of the air and the moisture of taking away reaction mass in the still; Exhaust again when reactor temperature is raised to 180 ~ 200 ℃, equipressure represent that number charges into the argon gas of 1.0～2MPa again when being down to zero;
(5) detonator burning when reactor temperature reaches 250 ℃～295 ℃, cause blank to carry out combustion synthesis reaction and discharge a large amount of heat, temperature of reaction kettle and pressure sharply raise, close the heating trip switch this moment, the reaction oneself keeps under self heat release condition, can obtain containing the block materials of ZrSi product after reaction is finished;
(6) block materials that contains ZrSi is cooled to room temperature with reactor in argon shield, uses crusher that its grinding is powder, leaches processing with hydrochloric acid, and extraction time is 48～96h;
(7) ZrSi after will leaching separates with leach liquor, uses distilled water wash ZrSi, is used for removing residual hydrochloric acid and sodium-chlor, and final drying 24h obtains target ZrSi powder, and its content is 97～99wt.%, granularity 269 ~ 320nm.
The invention has the beneficial effects as follows that production operation is simple, energy loss is little, obtains the high ultra-fine ZrSi powder of purity with low-cost, can fire feather weight block product at every turn, is suitable for suitability for industrialized production.Compare present method with other preparation methods following 2 improvement arranged:
(1) cost is low.Magnesium powder, zirconium white and silica flour with cheapness are reaction raw materials; The burning generated time of reaction is short, and the heat oneself who is discharged by thermopositive reaction self in reaction process keeps reaction and carry out, and namely no longer needs external energy to supply with after reaction is lighted; Production operation and impurity removal process are simple, have simplified production unit, have reduced cost.
(2) productive rate height.Combustion synthesis reaction of the present invention carries out in the 40L reactor, and the reaction mass total amount can be synthesized the ZrSi powder quality more than 1 kilogram more than 2 kilograms at every turn.
Embodiment
The present invention isA kind of preparation method of ultra-fine ZrSi powder the steps include:
(1) by mass percentage, according to Mg:84.36～108.46, ZrO
2: 216.31～278.12, prepare burden in Si:49.31～63.40, NaCl:50.00～150.00;
(2) the good raw material of weighing carries out ball milling, and time remaining 8～12h evenly mixes its powder;
(3) reaction mass mixes and is placed in the mould, and pressure-controlling is pressed into reaction mass the round pie blank under 10～20MPa; In reactor, put the tablet detonator in the copper crucible, again the blank that suppresses is placed on the detonator;
(4) sealed reactor at room temperature charges into 0.5～1.5MPa argon gas in reactor, open reactor heating trip switch then, is warming up to 120 ℃ of exhausts, to get rid of the air and the moisture of taking away reaction mass in the still; Exhaust again when reactor temperature is raised to 180 ~ 200 ℃, equipressure represent that number charges into the argon gas of 1.0～2MPa again when being down to zero;
(5) detonator burning when reactor temperature reaches 250 ℃～295 ℃, cause blank to carry out combustion synthesis reaction and discharge a large amount of heat, temperature of reaction kettle and pressure sharply raise, close the heating trip switch this moment, the reaction oneself keeps under self heat release condition, can obtain containing the block materials of ZrSi product after reaction is finished;
(6) block materials that contains ZrSi is cooled to room temperature with reactor in argon shield, uses crusher that its grinding is powder, leaches processing with hydrochloric acid, and extraction time is 48～96h;
(7) ZrSi after will leaching separates with leach liquor, uses distilled water wash ZrSi, is used for removing residual hydrochloric acid and sodium-chlor, and final drying 24h obtains target ZrSi powder, and its content is 97～99wt.%, granularity 269 ~ 320nm.
Further launch the present invention with embodiment below.
Embodiment 1:
Prepare Mg:96.5, ZrO by mass percentage
2: 278.12, Si:63.40, NaCl:50.00 reaction raw materials, be placed on then in the ball grinder, ball-milling medium is Al
2O
3Ball, ball material mass ratio is 1:2, is to be even mixed powder raw material on the planetary ball mill of 8h the 100r/min ball milling time at rotating speed.The reaction raw materials that mixes is placed mould, under the pressure of 10MPa, with pressing machine it is pressed into the round pie blank; Place the tablet detonator in reactor in the copper crucible, the blank after will making again places on the detonator; Sealed reactor charges into the 0.5MPa argon gas in the still, open heater switch, discharges gas reactor after waiting to be warming up to 120 ℃, is used for removing air in the still and takes away the moisture of reaction raw materials; Exhaust again when temperature in the kettle is raised to 180 ℃ charges into the argon gas of 1MPa then; The detonator burning causes blank generation combustion synthesis reaction when temperature in the kettle reaches 250 ℃, and temperature of reaction kettle and pressure sharply raise, and can close heater switch this moment; The reaction oneself keeps under self heat release condition, can obtain containing the block materials of ZrSi product after reaction is finished.After containing the block materials taking-up of ZrSi, use crusher that it is ground and be powder, (9.3mol/L) leaches 72h with powder with hydrochloric acid, ZrSi after will leaching with vacuum pump separates with leach liquor, with the ZrSi in the distilled water wash B, be used for removing residual hydrochloric acid and sodium-chlor, final drying 24h obtains the ZrSi powder body material, its content is 97.25wt.%, and granularity is that 0.1 ~ 0.9 μ m average particle size particle size is 0.32 μ m.
Embodiment 2:
Prepare Mg:108.46, ZrO by mass percentage
2: 247.21, Si:56.36, NaCl:100.00 reaction raw materials, be placed on then in the ball grinder, ball-milling medium is Al
2O
3Ball, ball material mass ratio is 1:2.5, is to be even mixed powder raw material on the planetary ball mill of 10h the 120r/min ball milling time at rotating speed.The reaction raw materials that mixes is placed mould, under the pressure of 15MPa, with pressing machine it is pressed into the round pie blank; Place the tablet detonator in reactor in the copper crucible, the blank after will making again places on the detonator; Sealed reactor charges into the 1MPa argon gas in the still, open heater switch, discharges gas reactor after waiting to be warming up to 120 ℃, is used for removing air in the still and takes away the moisture of reaction raw materials; Exhaust again when temperature in the kettle is raised to 190 ℃ charges into the argon gas of 1.5MPa then; The detonator burning causes blank generation combustion synthesis reaction when temperature in the kettle reaches 265 ℃, and temperature of reaction kettle and pressure sharply raise, and can close heater switch this moment; The reaction oneself keeps under self heat release condition, can obtain containing the block materials of ZrSi product after reaction is finished.After containing the block materials taking-up of ZrSi, use crusher that it is ground and be powder, (9.6mol/L) leaches 80h with powder with hydrochloric acid, ZrSi after will leaching with vacuum pump separates with leach liquor, with the ZrSi in the distilled water wash B, be used for removing residual hydrochloric acid and sodium-chlor, final drying 24h obtains the ZrSi powder body material, its content is 98.03wt.%, and granularity is that 0.1 ~ 0.7 μ m average particle size particle size is 0.29 μ m.
Embodiment 3:
Prepare Mg:84.36, ZrO by mass percentage
2: 216.31, Si:49.31, NaCl:150.00 reaction raw materials, be placed on then in the ball grinder, ball-milling medium is Al
2O
3Ball, ball material mass ratio is 1:3, is to be even mixed powder raw material on the planetary ball mill of 12h the 150r/min ball milling time at rotating speed.The reaction raw materials that mixes is placed mould, under the pressure of 20MPa, with pressing machine it is pressed into the round pie blank; Place the tablet detonator in reactor in the copper crucible, the blank after will making again places on the detonator; Sealed reactor charges into the 1.5MPa argon gas in the still, open heater switch, discharges gas reactor after waiting to be warming up to 120 ℃, is used for removing air in the still and takes away the moisture of reaction raw materials; Exhaust again when temperature in the kettle is raised to 200 ℃ charges into the argon gas of 2MPa then; The detonator burning causes blank generation combustion synthesis reaction when temperature in the kettle reaches 275 ℃, and temperature of reaction kettle and pressure sharply raise, and can close heater switch this moment; The reaction oneself keeps under self heat release condition, can obtain containing the block materials of ZrSi product after reaction is finished.After containing the block materials taking-up of ZrSi, use crusher that it is ground and be powder, (11.6mol/L) leaches 96h with powder with hydrochloric acid, ZrSi after will leaching with vacuum pump separates with leach liquor, with the ZrSi in the distilled water wash B, be used for removing residual hydrochloric acid and sodium-chlor, final drying 24h obtains the ZrSi powder body material, its content is 98.78wt.%, and granularity is that 0.1 ~ 0.5 μ m average particle size particle size is 0.26 μ m.
Claims (3)
1. the preparation method of a ultra-fine ZrSi powder the steps include:
(1) by mass percentage, according to Mg:84.36～108.46, ZrO
2: 216.31～278.12, prepare burden in Si:49.31～63.40, NaCl:50.00～150.00;
(2) the good raw material of weighing carries out ball milling, and time remaining 8～12h evenly mixes its powder;
(3) reaction mass mixes and is placed in the mould, and pressure-controlling is pressed into reaction mass the round pie blank under 10～20MPa; In reactor, put the tablet detonator in the copper crucible, again the blank that suppresses is placed on the detonator;
(4) sealed reactor at room temperature charges into 0.5～1.5MPa argon gas in reactor, open reactor heating trip switch then, is warming up to 120 ℃ of exhausts, to get rid of the air and the moisture of taking away reaction mass in the still; Exhaust again when reactor temperature is raised to 180 ~ 200 ℃, equipressure represent that number charges into the argon gas of 1.0～2MPa again when being down to zero;
(5) detonator burning when reactor temperature reaches 250 ℃～295 ℃, cause blank to carry out combustion synthesis reaction and discharge a large amount of heat, temperature of reaction kettle and pressure sharply raise, close the heating trip switch this moment, the reaction oneself keeps under self heat release condition, can obtain containing the block materials of ZrSi product after reaction is finished;
(6) block materials that contains ZrSi is cooled to room temperature with reactor in argon shield, uses crusher that its grinding is powder, leaches processing with hydrochloric acid, and extraction time is 48～96h;
(7) ZrSi after will leaching separates with leach liquor, uses distilled water wash ZrSi, is used for removing residual hydrochloric acid and sodium-chlor, and final drying 24h obtains target ZrSi powder, and its content is 97～99wt.%, granularity 269 ~ 320nm.
2.
According to claim 1The preparation method of ultra-fine ZrSi powder is characterized in that: the good raw material of weighing is with in its ball grinder of packing into, and ball milling 8～12h on planetary ball mill evenly mixes its powder, and rotating speed is 50～150r/min, and ball material mass ratio is 1:2～1:3, and ball-milling medium is Al
2O
3Ball.
3.
According to claim 1The preparation method of ultra-fine ZrSi powder is characterized in that: be that the hydrochloric acid of 8～11.6mol/L leaches processing with concentration.
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|---|---|---|---|
| CN2013102351987A CN103253675A (en) | 2013-06-14 | 2013-06-14 | Preparation method of superfine ZrSi powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156025A (en) * | 2019-05-27 | 2019-08-23 | 吉林大学 | A kind of preparation method of the metal silicide of pure phase |
| CN111592000A (en) * | 2020-05-14 | 2020-08-28 | 江苏理工学院 | Method for preparing zirconium silicide nano material |
| CN111825096A (en) * | 2020-07-23 | 2020-10-27 | 辽宁中色新材科技有限公司 | Method for producing zirconium disilicide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1555088A (en) * | 2003-12-22 | 2004-12-15 | 西安交通大学 | Nano double phase composite structure Zr-Si-N diffusion barrier material and its preparing process |
| CN102344149A (en) * | 2011-06-16 | 2012-02-08 | 兰州理工大学 | Preparation method of ZrB2 powder material |
-
2013
- 2013-06-14 CN CN2013102351987A patent/CN103253675A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1555088A (en) * | 2003-12-22 | 2004-12-15 | 西安交通大学 | Nano double phase composite structure Zr-Si-N diffusion barrier material and its preparing process |
| CN102344149A (en) * | 2011-06-16 | 2012-02-08 | 兰州理工大学 | Preparation method of ZrB2 powder material |
Non-Patent Citations (1)
| Title |
|---|
| HONG YOUL RYU ET AL: "Preparation of zirconium-based ceramic and composite fine-grained powders", 《INT.JOURNAL OF REFRACTORY METALS AND HARD MATERIALS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156025A (en) * | 2019-05-27 | 2019-08-23 | 吉林大学 | A kind of preparation method of the metal silicide of pure phase |
| CN110156025B (en) * | 2019-05-27 | 2021-07-20 | 吉林大学 | Preparation method of pure-phase metal silicide |
| CN111592000A (en) * | 2020-05-14 | 2020-08-28 | 江苏理工学院 | Method for preparing zirconium silicide nano material |
| CN111825096A (en) * | 2020-07-23 | 2020-10-27 | 辽宁中色新材科技有限公司 | Method for producing zirconium disilicide |
| CN111825096B (en) * | 2020-07-23 | 2022-05-31 | 辽宁中色新材科技有限公司 | Method for producing zirconium disilicide |
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Application publication date: 20130821 |