CN102765946B - Current assisted method for quickly preparing powder - Google Patents
Current assisted method for quickly preparing powder Download PDFInfo
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- CN102765946B CN102765946B CN 201210232519 CN201210232519A CN102765946B CN 102765946 B CN102765946 B CN 102765946B CN 201210232519 CN201210232519 CN 201210232519 CN 201210232519 A CN201210232519 A CN 201210232519A CN 102765946 B CN102765946 B CN 102765946B
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Abstract
The invention provides a current assisted method for quickly preparing powder. A current assisted device for quickly preparing powder is adopted. A reaction cavity of the device is a sealed space enclosed by a side wall and the upper and lower end covers of the cavity. The upper and lower end covers are respectively connected with pressure heads of the upper and lower electrodes. In a work state, pressure generated by the pressure heads of the upper and lower electrodes is borne by the side wall and the upper and lower end covers of the cavity. The volume of the sealed space is invariable. The method comprises the steps of: first, placing the powder in the reaction cavity; then, connecting a direct current or a high frequency pulse current between the pressure heads of the upper and lower electrodes, wherein the current generates heat through the reaction cavity and the powder is heated quickly; measuring temperature of the reaction cavity through a temperature measuring part; shutting down the current when the temperature rises the predetermined temperature and is maintained for a period of time; and taking out the powder after the cavity is cooled. According to the method provided by the invention, the current assisted sintering principle is combined into a powder preparation process, and powder such as metal, ceramic and the like can be rapidly prepared conveniently and quickly, so that the method provided by the invention has good application prospect.
Description
Technical field
The present invention relates to the Preparation Technique of Powders fields such as metal, pottery, relate in particular to a kind of auxiliary method for preparing fast powder of electric current.
Background technology
Electric current assisted sintering technology (EAST) is to utilize DC current or high-frequency pulse current to realize being rapidly heated, and the sintering process of high thermal efficiency is exerted pressure to realize in the electrode two ends simultaneously.This sintering processing claims again electric field assisted sintering (EFS), electric field activated sintering (EAS), pulse current activation pressure sintering (PECPS) and discharge plasma sintering (SPS) etc.
At present, can realize the device of electric current assisted sintering technology as shown in Figure 1, mainly comprise the reaction cavity 1 for placing material to be sintered, the upper/lower electrode pressure head 2 and 3 that is arranged on reaction cavity 1 two ends, by input direct-current electric current or high-frequency pulse current, reaction cavity 1 is rapidly heated, and be positioned on reaction cavity 1, for placing the thermometer hole 4 of temperature-measuring part with monitoring reaction cavity 1 temperature; Wherein, as shown in Figure 2, reaction cavity 1 is the enclosure space surrounded by cavity wall 7, upper end cover 5 and bottom end cover 6, upper end cover 5 is connected with top electrode pressure head 2, bottom end cover 6 is connected with bottom electrode pressure head 3, and upper end cover 5 is or/and bottom end cover 6 can be along the cavity wall upper and lower displacement, the volume of described enclosure space with upper end cover 5 or/and the upper and lower displacement of bottom end cover 6 change.This installs when in running order, the question response material is placed in reaction cavity 1, input direct-current electric current or high-frequency pulse current between top electrode pressure head 2 and bottom electrode pressure head 3, reaction cavity 1 is rapidly heated, simultaneously upper end cover 5 and bottom end cover 6 due to bear top electrode pressure head 2 with the load of bottom electrode pressure head 3 along cavity wall downwards with to top offset, not only treat reaction material and realized sintering process, also it has been realized to mould pressing process.Therefore, this device is applicable to realize the quick densifying of metal, ceramic material, especially having unique advantage for block materials such as realizing nanocrystalline ceramics, superhigh temperature structural ceramics, texturing function and structural ceramics, thermoelectricity functional material, intermetallic compound, carbide alloy, high-performance metal target material, glass-metal material, nonequilibrium state solid material, is the quantum jump in sintering technology field in recent years.
This seminar is explored on basis in long-term scientific research, in conjunction with current application, need, propose recently, electric current assisted sintering technology is used in to the Preparation Technique of Powders fields such as metal, pottery, make powder experience the processes such as phase transformation, solid phase reaction in electric current assisted sintering process, thereby obtain required powder.But, while adopting above-mentioned electric current assisted sintering device to carry out sintering to powder, design feature due to current reaction cavity, although powder has experienced the processes such as phase transformation, solid phase reaction in sintering process, finally but can only obtain full densification or the fine and close block of part that sintering forms, but not keep former powder morphology.
Summary of the invention
Technical purpose of the present invention is for utilizing above-mentioned electric current assisted sintering device can only obtain the deficiency of block materials, a kind of method for preparing fast powder is provided, the method, based on electric current assisted sintering principle, can realize the quick preparation of the powders such as metal, pottery quickly and easily.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is: a kind of auxiliary method for preparing fast powder of electric current, the method adopts the auxiliary quick powder preparation facilities of electric current, the auxiliary quick powder preparation facilities of this electric current comprises the reaction cavity for placing powder, the upper and lower electrode pressure head that is arranged on the reaction cavity two ends, by input direct-current electric current or high-frequency pulse current, reaction cavity is rapidly heated, and be positioned on reaction cavity, for placing the thermometer hole of temperature-measuring part with monitoring reaction cavity temperature; Wherein, reaction cavity is the enclosure space surrounded by cavity wall, upper end cover and bottom end cover, upper end cover is connected with the top electrode pressure head, bottom end cover is connected with the bottom electrode pressure head, in the time of in working order, the pressure that top electrode pressure head and bottom electrode pressure head produce is born by cavity wall, upper end cover and bottom end cover, and the volume of the enclosure space that described cavity wall, upper end cover and bottom end cover surround immobilizes;
The method specifically comprises the steps;
In technique scheme:
As preferably, the cross section of a certain position of described upper end cover is greater than the reaction cavity diameter, can make upper end cover be buckled in cavity wall top, the cross section of a certain position of bottom end cover is greater than the reaction cavity diameter, can make bottom end cover be buckled in the cavity wall bottom, thereby keep the volume of enclosure space to immobilize;
Preferred as another kind, described bottom end cover and cavity wall are combined as a whole, and the cross section of a certain position of upper end cover is greater than the reaction cavity diameter, can make upper end cover be buckled in cavity wall top, thereby keep the volume of enclosure space to immobilize;
The shape of the enclosure space that described cavity wall, upper end cover and bottom end cover surround is not limit, and includes but not limited to cylindrically, and cross section is rectangle, square, triangle, trapezoidal, other are regular or erose column structure;
Described cavity wall, upper end cover and bottom end cover are made by the high-melting-point conductive material respectively, include but not limited to be made by graphite material;
As preferably, described thermometer hole is arranged on upper end cover or bottom end cover position;
As preferably, described temperature-measuring part is upper infrared radiation thermometer; Described temperature-measuring part is directly measured the temperature of powder in reaction cavity, or measures the temperature on reaction cavity surface;
Produce pollution for fear of being spread in reaction cavity by powder, preferably, in described step 1, powder is placed in conduction or nonconducting crucible, crucible is placed in reaction cavity.
In sum, the invention provides a kind of auxiliary method for preparing fast powder of electric current, the auxiliary quick powder preparation facilities of the electric current that the method adopts is to be improved and obtained by the existing electric current assisted sintering device prepared for block, will be by cavity wall, the reaction cavity of the sealing that the volume that upper end cover and bottom end cover surround is adjustable is improved to by cavity wall, upper end cover and bottom end cover bear the contact of upper/lower electrode pressure head, and the changeless reaction cavity structure of maintenance enclosure space volume, thereby can be by being rapidly heated of direct current or high-frequency pulse current realization response cavity be provided, thereby realize metal, the auxiliary Fast Sintering of the electric current of the powders such as pottery, there is following advantage:
(1) by being rapidly heated of direct current or high-frequency pulse current realization response cavity is provided, provide powder to react required thermal environment, be conducive to that powder is rapidly heated, fast reaction, greatly shortened powder and prepared required time;
(2) can obtain the arbitrary temp in 400～2200 degrees centigrade, heating rate is controlled in 1～400 degrees celsius/minute, can adopt inert atmosphere and reaction atmosphere, and can realize condition of high vacuum degree;
(3) be applicable to conduction, non-conductive powder or hybrid conductive powder;
For non-conductive powder, powder is among the reaction cavity internal electric field; For conductive powder or hybrid conductive powder, the electric current that electric current assisted sintering device provides is at the reaction cavity powder of flowing through, with electric field (electric current) coupling of powder generation, thereby solid phase reaction is produced to special effect, further realize low temperature, powder reaction fast;
(4) simplicity of design, practicality can realize on the basic structure of existing electric current assisted sintering equipment in transformation, have expanded the function of electric current assisted sintering equipment, and can realize the quick preparation of powder;
(5) utilize the auxiliary quick powder preparation facilities of this electric current can carry out kinds of processes prepared by powder, comprise powder heat treatment (annealing and normalizing), solid-state phase changes, solid phase reaction is synthetic, the solid and gas two phase reaction is synthetic etc.
The accompanying drawing explanation
Fig. 1 is existing electric current assisted sintering device schematic diagram;
Fig. 2 is the reaction cavity structural representation in Fig. 1;
To be that in the embodiment of the present invention 1, electric current is auxiliary prepare the apparatus structure schematic diagram that powder adopts to Fig. 3 fast;
Fig. 4 is the auxiliary vertical section structure schematic diagram for preparing fast reaction cavity in the device that powder adopts of electric current in the embodiment of the present invention 1;
Fig. 5 is the auxiliary vertical section structure schematic diagrames that prepare fast reaction cavity in the device that powder adopts of the embodiment of the present invention 2 electric currents.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and it is not played to any restriction effect.
The drawing reference numeral of Fig. 1 to Fig. 5 is: 1, reaction cavity, 2, the top electrode pressure head, 3, the bottom electrode pressure head, 4, thermometer hole, 5, upper end cover, 6, bottom end cover, 7, cavity wall.
Embodiment 1:
In the present embodiment, electric current assists the method for preparing fast powder specific as follows:
Adopt the auxiliary quick powder preparation facilities of electric current, the structural representation of this device as shown in Figure 3, comprises the reaction cavity 1 for placing powder, the upper/lower electrode pressure head 2 and 3 be connected with reaction cavity 1.Reaction cavity 1 is the enclosure space surrounded by cavity wall 7, upper end cover 5 and bottom end cover 6, and upper end cover 5 is connected with top electrode pressure head 2, and bottom end cover 6 is connected with bottom electrode pressure head 3, and the volume of this enclosure space is fixed.On upper end cover 5, arranging for placing the thermometer hole 4 of temperature-measuring part with monitoring reaction cavity 1 interior temperature, this temperature-measuring part is selected infrared radiation thermometer.As shown in Figure 4, the cross section of a certain position of upper end cover 5 is greater than the diameter of reaction cavity 1, can make upper end cover 6 be buckled in the top of cavity wall 7.The cross section of a certain position of bottom end cover 6 is greater than the diameter of reaction cavity 1, can make bottom end cover 6 be buckled in the bottom of cavity wall 7, thereby keep the volume of enclosure space to immobilize.Cavity wall 7, upper end cover 5 select respectively graphite material to make with bottom end cover 6.In the time of in working order, top electrode pressure head 2 is born with bottom end cover 6 by cavity wall 7, upper end cover 5 with the pressure that bottom electrode pressure head 3 produces, and the volume of the enclosure space that described cavity wall 7, upper end cover 5 and bottom end cover 6 surround immobilizes, avoid pressure directly to be loaded on powder.
The method of utilizing the auxiliary quick powder preparation facilities of above-mentioned electric current to prepare powder comprises the steps:
1, open reaction cavity 1, can place conduction or non-conductive crucible in reaction cavity 1 inside, powder is placed in crucible;
2, the off-response cavity 1, keep the enclosure space volume of reaction cavity to immobilize, directly connect direct current or high-frequency pulse current at top electrode pressure head 2 and bottom electrode pressure head 3, electric current produces heat by reaction cavity, provide powder to react required thermal environment, being rapidly heated of realization response cavity 1, programming rate is controlled by direct current or high-frequency pulse current size;
Measure the temperature of reaction cavity 1 interior powder by upper infrared radiation thermometer, powder heats up according to preset temperature, until powder, reaches required heating-up temperature and, after this temperature is incubated the corresponding time, completes the heating preparation process of powder;
3, close current, open reaction cavity, takes out powder.
Embodiment 2:
In the present embodiment, electric current assists the method for preparing fast powder specific as follows:
Adopt the auxiliary quick powder preparation facilities of electric current, the structural representation of this device is as shown in Figure 3 similar, comprises the reaction cavity 1 for placing powder, the upper/lower electrode pressure head 2 and 3 be connected with reaction cavity 1.Reaction cavity 1 is the enclosure space surrounded by cavity wall 7, upper end cover 5 and bottom end cover 6, and upper end cover 5 is connected with top electrode pressure head 2, and bottom end cover 6 is connected with bottom electrode pressure head 3, and the volume of this enclosure space is fixed.On upper end cover 5, arranging for placing the thermometer hole 4 of temperature-measuring part with monitoring reaction cavity 1 interior temperature, this temperature-measuring part is selected infrared radiation thermometer.As shown in Figure 5, bottom end cover 6 is combined as a whole with cavity wall 7, and the cross section of upper end cover 5 a certain positions is greater than reaction cavity 1 diameter, can make upper end cover 5 be buckled in the top of cavity wall 7, thereby keep the volume of enclosure space to immobilize.Cavity wall 7, upper end cover 5 select respectively graphite material to make with bottom end cover 6.In the time of in working order, top electrode pressure head 2 is born with bottom end cover 6 by cavity wall 7, upper end cover 5 with the pressure that bottom electrode pressure head 3 produces, and the volume of the enclosure space that described cavity wall 7, upper end cover 5 and bottom end cover 6 surround immobilizes, avoid pressure directly to be loaded on powder.
The method of utilizing the auxiliary quick powder preparation facilities of above-mentioned electric current to prepare powder comprises the steps:
1, open reaction cavity 1, can place conduction or non-conductive crucible in reaction cavity 1 inside, powder is placed in crucible;
2, the off-response cavity 1, keep the enclosure space volume of reaction cavity to immobilize, directly connect direct current or high-frequency pulse current at top electrode pressure head 2 and bottom electrode pressure head 3, electric current produces heat by reaction cavity, provide powder to react required thermal environment, being rapidly heated of realization response cavity 1, programming rate is controlled by direct current or high-frequency pulse current size;
Measure the temperature of reaction cavity 1 interior powder by upper infrared radiation thermometer, powder heats up according to preset temperature, until powder, reaches required heating-up temperature and, after this temperature is incubated the corresponding time, completes the heating preparation process of powder;
3, close current, open reaction cavity, takes out powder.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making in principle scope of the present invention, supplement or similar fashion substitutes etc., within all should being included in protection scope of the present invention.
Claims (6)
1. the auxiliary method for preparing fast powder of electric current, is characterized in that: adopt the auxiliary quick powder preparation facilities of electric current to complete in accordance with the following steps;
The auxiliary quick powder preparation facilities of described electric current comprises the reaction cavity (1) for placing powder, top electrode pressure head (2) and the bottom electrode pressure head (3) that is arranged on reaction cavity (1) two ends, by input direct-current electric current or high-frequency pulse current, reaction cavity (1) is rapidly heated, and be positioned at reaction cavity (1) upper, for placing the thermometer hole (4) of temperature-measuring part with monitoring reaction cavity (1) temperature, it is characterized in that: described reaction cavity (1) is by cavity wall (7), the enclosure space that upper end cover (5) and bottom end cover (6) surround, cavity wall (7), upper end cover (5) is made by graphite material respectively with bottom end cover (6), upper end cover (5) is connected with top electrode pressure head (2), bottom end cover (6) is connected with bottom electrode pressure head (3), during duty, the pressure that top electrode pressure head (2) and bottom electrode pressure head (3) produce is by cavity wall (7), upper end cover (5) bears with bottom end cover (6), the volume of described enclosure space immobilizes,
Step 1, at inner conduction or the non-conductive crucible placed of reaction cavity (1), powder is placed in crucible, keep the enclosure space volume of reaction cavity (1) to immobilize;
Step 2, at top electrode pressure head (2) and the indirect perfectly straight stream of bottom electrode pressure head (3) or high-frequency pulse current, electric current produces heat by reaction cavity (1), reaction cavity (1) heats up, the powder be placed in reaction cavity (1) heats up thereupon, and programming rate is controlled by direct current or high-frequency pulse current size;
Step 3, by temperature-measuring part, measure the temperature in reaction cavity (1), until powder, reach required heating-up temperature and, after this temperature insulation certain hour, complete the heating preparation process of powder;
Step 4, close current, after question response cavity (1) is cooling, take out powder.
2. electric current according to claim 1 is assisted the method for preparing fast powder, it is characterized in that: the cross section of a certain position of described upper end cover (5) is greater than reaction cavity (1) diameter, make upper end cover (5) be buckled in cavity wall (7) top, the cross section of a certain position of bottom end cover (6) is greater than reaction cavity (1) diameter, makes bottom end cover (6) be buckled in cavity wall (7) bottom.
3. electric current according to claim 1 and 2 is assisted the method for preparing fast powder, it is characterized in that: described bottom end cover (6) is combined as a whole with cavity wall (7), the cross section of a certain position of upper end cover (5) is greater than reaction cavity (1) diameter, makes upper end cover (5) be buckled in cavity wall (7) top.
4. electric current according to claim 1 and 2 is assisted the method for preparing fast powder, and it is characterized in that: described thermometer hole (4) is arranged on upper end cover (5) or bottom end cover (6) position.
5. electric current according to claim 1 and 2 is assisted the method for preparing fast powder, and it is characterized in that: the temperature of described reaction cavity (1) is controlled at 400～2200 degrees centigrade, and heating rate is controlled at 1～400 degrees celsius/minute.
6. the auxiliary method for preparing fast powder of electric current according to claim 1 and 2 is characterized in that: the annealing that the heating preparation process of described powder comprises powder and normalizing heat treatment, solid-state phase changes, the process that solid phase reaction is synthesized, the solid and gas two phase reaction is synthetic.
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| CN106197755B (en) * | 2016-08-22 | 2018-11-06 | 郑州磨料磨具磨削研究所有限公司 | Mold center's thermometry and hot-press sintering equipment |
| CN106077619A (en) * | 2016-08-23 | 2016-11-09 | 安徽华东光电技术研究所 | Metal dust high frequency annealing method |
| CN106238732B (en) * | 2016-08-30 | 2019-08-02 | 浙江晨华科技有限公司 | A kind of discharge plasma sintering system |
| CN106116559B (en) * | 2016-08-30 | 2018-12-25 | 西南交通大学 | A kind of electric field-assisted ceramic low-temp quick-combustion device |
| CN110078496A (en) * | 2018-01-25 | 2019-08-02 | 国家电投集团科学技术研究院有限公司 | The preparation method and preparation facilities of ceramic material |
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| CN110425877A (en) * | 2019-08-07 | 2019-11-08 | 清华大学深圳研究生院 | Ceramic post sintering device and ceramic post sintering method |
| CN114349005B (en) * | 2022-01-14 | 2023-06-09 | 天津大学 | Preparation method of high-entropy metal carbide ceramic powder |
| CN114951649B (en) * | 2022-06-21 | 2024-02-13 | 重庆三航新材料技术研究院有限公司 | Die for rapid smelting or vacuum heat treatment of discharge plasma and application method thereof |
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| JPH0221190A (en) * | 1988-07-07 | 1990-01-24 | Kobe Steel Ltd | High-temperature and high-pressure treatment device |
| JP3781072B2 (en) * | 1997-06-05 | 2006-05-31 | 石川島播磨重工業株式会社 | Sintering equipment |
| JPH11117006A (en) * | 1997-10-13 | 1999-04-27 | Inr Kenkyusho:Kk | Method and device for discharge sintering |
| KR100873467B1 (en) * | 2007-07-30 | 2008-12-15 | 한국생산기술연구원 | Method and apparatus of pressure-assisted electric-current sintering |
| EP2198993B1 (en) * | 2008-12-19 | 2012-09-26 | EPoS S.r.L. | Sintering process and corresponding sintering system |
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