CN102765946A - Current assisted method for quickly preparing powder - Google Patents
Current assisted method for quickly preparing powder Download PDFInfo
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- CN102765946A CN102765946A CN2012102325193A CN201210232519A CN102765946A CN 102765946 A CN102765946 A CN 102765946A CN 2012102325193 A CN2012102325193 A CN 2012102325193A CN 201210232519 A CN201210232519 A CN 201210232519A CN 102765946 A CN102765946 A CN 102765946A
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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 powder preparing technical fields such as metal, pottery, relate in particular to the auxiliary method for preparing powder fast of a kind of electric current.
Background technology
Electric current assisted sintering technology (EAST) is to utilize galvanic current or high-frequency pulse current to realize being rapidly heated, and exert pressure to realize the sintering process of high thermal efficiency in the electrode two ends simultaneously.This sintering processing is claimed electric field assisted sintering (EFS), electric field activated sintering (EAS), pulsed current activation pressure sintering (PECPS) and discharge plasma sintering (SPS) etc. again.
At present; The device that can realize electric current assisted sintering technology is as shown in Figure 1; The upper/lower electrode pressure head 2 and 3 that mainly comprises the reaction cavity 1 that is used to place material to be sintered, is arranged on reaction cavity 1 two ends, reaction cavity 1 is rapidly heated through input dc power stream or high-frequency pulse current, and be positioned on the reaction cavity 1, be used to place temperature-measuring part to monitor the thermometer hole 4 of reaction cavity 1 temperature; Wherein, As shown in Figure 2; Reaction cavity 1 is the enclosed space that is surrounded by cavity wall 7, upper end cover 5 and lower end cover 6, and upper end cover 5 is connected with top electrode pressure head 2, and lower end cover 6 is connected with lower electrode pressure head 3; And upper end cover 5 is or/and lower end cover 6 can be along the cavity wall upper and lower displacement, promptly the volume of said enclosed space with upper end cover 5 or/and the upper and lower displacement of lower end cover 6 change.This installs when in running order; The question response material is placed in the reaction cavity 1; Input dc power stream or high-frequency pulse current are rapidly heated reaction cavity 1 between top electrode pressure head 2 and the lower electrode pressure head 3, simultaneously upper end cover 5 with lower end cover 6 since bear top electrode pressure head 2 with the load of lower electrode pressure head 3 along cavity wall downwards with to top offset; Promptly not only treat reaction material and realized sintering process, also it has been realized mould pressing process.Therefore; This device is applicable to the quick densifying of realizing metal, stupalith; Especially having special advantages for block materials such as realizing nanocrystalline ceramics, ultrahigh-temperature structural ceramics, texturing function and structural ceramics, thermoelectric functional materials, intermetallic compound, wimet, 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 the basis in secular scientific research; In conjunction with present application need; Propose recently; Electric current assisted sintering technology is used in powder preparing technical fields such as metal, pottery, makes powder in electric current assisted sintering process, experience processes such as phase transformation, solid state reaction, thereby obtain required powder.But; When adopting above-mentioned electric current assisted sintering device that powder is carried out sintering; Because the constructional feature of present reaction cavity; Though powder has experienced processes such as phase transformation, solid state reaction in sintering process, finally 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 to utilizing above-mentioned electric current assisted sintering device can only obtain the deficiency of block materials; A kind of quick method for preparing powder is provided; This method can realize the quick preparation of powders such as metal, pottery quickly and easily based on electric current assisted sintering principle.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is: the auxiliary method for preparing powder fast of a kind of electric current; This method adopts the auxiliary quick powder preparing device of electric current; The upper and lower electrode pressure head that the auxiliary quick powder preparing device of this electric current comprises the reaction cavity that is used to place powder, is arranged on the reaction cavity two ends, reaction cavity is rapidly heated through input dc power stream or high-frequency pulse current, and be positioned on the reaction cavity, be used to place the thermometer hole of temperature-measuring part with monitoring reaction cavity temperature; Wherein, Reaction cavity is the enclosed space that is surrounded by cavity wall, upper end cover and lower end cover; Upper end cover is connected with the top electrode pressure head, and lower end cover is connected with the lower electrode pressure head, in the time of in working order; The pressure that top electrode pressure head and lower electrode pressure head produce is born by cavity wall, upper end cover and lower end cover, and the volume of the enclosed space that described cavity wall, upper end cover and lower end cover surrounded immobilizes;
This method specifically comprises the steps;
In the technique scheme:
As preferably; The xsect 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 xsect of a certain position of lower end cover can make lower end cover be buckled in the cavity wall bottom greater than the reaction cavity diameter, thereby keeps the volume of enclosed space to immobilize;
Preferred as another kind, described lower end cover and cavity wall are combined as a whole, and the xsect of a certain position of upper end cover can make upper end cover be buckled in cavity wall top greater than the reaction cavity diameter, thereby keep the volume of enclosed space to immobilize;
The shape of the enclosed space that described cavity wall, upper end cover and lower end cover surround is not limit, include but not limited to cylindrical, xsect be rectangle, square, trilateral, trapezoidal, other are regular or erose column structure;
Described cavity wall, upper end cover and lower end cover are processed by the HMP electro-conductive material respectively, include but not limited to processed by graphite material;
As preferably, described thermometer hole is arranged on upper end cover or lower end cover position;
As preferably, described temperature-measuring part is last infrared thermometer; Described temperature-measuring part is directly measured the temperature of powder in the reaction cavity, perhaps measures the temperature on reaction cavity surface;
Produce pollution for fear of in reaction cavity, spreading, preferably in described step 1, powder is placed in conduction or the nonconducting crucible, crucible is placed in the reaction cavity by powder.
In sum; The invention provides the auxiliary method for preparing powder fast of a kind of electric current; The auxiliary quick powder preparing device of the electric current that this method adopted is to be improved by the existing electric current assisted sintering device that is used for the block preparation to obtain; To be improved to the contact pressure of bearing the upper/lower electrode pressure head by cavity wall, upper end cover and lower end cover by the reaction cavity of the adjustable sealing of the volume that cavity wall, upper end cover and lower end cover surround; And the changeless reaction cavity structure of maintenance enclosed space volume; Thereby can be through being rapidly heated of direct current or high-frequency pulse current realization response cavity be provided, thus realize the auxiliary Fast Sintering of electric current of powders such as metal, pottery, have following advantage:
(1) through being rapidly heated of direct current or high-frequency pulse current realization response cavity is provided, provide the powder reaction required thermal environment, help that powder is rapidly heated, rapid reaction, shortened the powder preparing required time greatly;
(2) can obtain arbitrary temp in 400～2200 degrees centigrade, temperature rise 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 state reaction is produced special effect, further realize low temperature, powder reaction fast;
(4) simplicity of design, practicality can be transformed on the substruction of existing electric current assisted sintering equipment and realized, have expanded the function of electric current assisted sintering equipment, and can realize the quick preparation of powder;
(5) utilize the auxiliary quick powder preparing device of this electric current can carry out the kinds of processes of powder preparing, comprise powder thermal treatment (annealing and normalizing), solid-state phase changes, solid state reaction is synthetic, the solid and gas two phase reaction is synthetic etc.
Description of drawings
Fig. 1 is existing electric current assisted sintering device synoptic diagram;
Fig. 2 is the reaction cavity structural representation among Fig. 1;
Fig. 3 is the auxiliary preparation fast of the electric current apparatus structure synoptic diagram that powder adopted in the embodiment of the invention 1;
Fig. 4 is the auxiliary vertical section structure synoptic diagram for preparing reaction cavity in the device that powder adopted fast of electric current in the embodiment of the invention 1;
Fig. 5 is the vertical section structure synoptic diagram of reaction cavity in the auxiliary preparation fast of the embodiment of the invention 2 electric currents device that powder adopted.
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 understanding of the present invention, and it is not played any qualification effect.
The drawing reference numeral of Fig. 1 to Fig. 5 is: 1, reaction cavity, 2, the top electrode pressure head, 3, the lower electrode pressure head, 4, thermometer hole, 5, upper end cover, 6, lower end cover, 7, cavity wall.
Embodiment 1:
In the present embodiment, electric current assists the method for preparing powder fast specific as follows:
Adopt the auxiliary quick powder preparing device of electric current, the structural representation of this device is as shown in Figure 3, comprises the reaction cavity 1 that is used to place powder, the upper/lower electrode pressure head 2 and 3 that links to each other with reaction cavity 1.Reaction cavity 1 is the enclosed space that is surrounded by cavity wall 7, upper end cover 5 and lower end cover 6, and upper end cover 5 is connected with top electrode pressure head 2, and lower end cover 6 is connected with lower electrode pressure head 3, and the volume of this enclosed space is fixed.Be provided with on the upper end cover 5 and be used to place the thermometer hole 4 of temperature-measuring part with temperature in the monitoring reaction cavity 1, this temperature-measuring part is selected infrared thermometer for use.As shown in Figure 4, the xsect of a certain position of upper end cover 5 can make upper end cover 6 be buckled in the top of cavity wall 7 greater than the diameter of reaction cavity 1.The xsect of a certain position of lower end cover 6 can make lower end cover 6 be buckled in the bottom of cavity wall 7, thereby keep the volume of enclosed space to immobilize greater than the diameter of reaction cavity 1.Cavity wall 7, upper end cover 5 select for use graphite material to process respectively with lower end cover 6.In the time of in working order; Top electrode pressure head 2 is born with lower end cover 6 by cavity wall 7, upper end cover 5 with the pressure that lower electrode pressure head 3 produces; And described cavity wall 7, upper end cover 5 immobilize with the volume of the enclosed space that lower end cover 6 is surrounded, and avoid pressure directly to be loaded on powder.
The method of utilizing the auxiliary quick powder preparing device of above-mentioned electric current to prepare powder comprises the steps:
1, opens reaction cavity 1, can place conduction or non-conductive crucible in reaction cavity 1 inside, powder is placed in the crucible;
2, the off-response cavity 1; Keep the enclosed space volume of reaction cavity to immobilize; Directly connect direct current or high-frequency pulse current at top electrode pressure head 2 and lower electrode pressure head 3, electric current produces heat through reaction cavity, provides the powder reaction required thermal environment; Being rapidly heated of realization response cavity 1, heat-up rate is by direct current or the control of high-frequency pulse current size;
Measure the temperature of powder in the reaction cavity 1 through last infrared thermometer, powder heats up according to preset temp, treats that powder reaches required Heating temperature and after this temperature is incubated the corresponding time, and that accomplishes powder adds the hot preparation process;
3, close current is opened reaction cavity, takes out powder.
Embodiment 2:
In the present embodiment, electric current assists the method for preparing powder fast specific as follows:
Adopt the auxiliary quick powder preparing device of electric current, the structural representation of this device is similar as shown in Figure 3, comprises the reaction cavity 1 that is used to place powder, the upper/lower electrode pressure head 2 and 3 that links to each other with reaction cavity 1.Reaction cavity 1 is the enclosed space that is surrounded by cavity wall 7, upper end cover 5 and lower end cover 6, and upper end cover 5 is connected with top electrode pressure head 2, and lower end cover 6 is connected with lower electrode pressure head 3, and the volume of this enclosed space is fixed.Be provided with on the upper end cover 5 and be used to place the thermometer hole 4 of temperature-measuring part with temperature in the monitoring reaction cavity 1, this temperature-measuring part is selected infrared thermometer for use.As shown in Figure 5, lower end cover 6 is combined as a whole with cavity wall 7, and the xsect of upper end cover 5 a certain positions can make upper end cover 5 be buckled in the top of cavity wall 7, thereby keep the volume of enclosed space to immobilize greater than reaction cavity 1 diameter.Cavity wall 7, upper end cover 5 select for use graphite material to process respectively with lower end cover 6.In the time of in working order; Top electrode pressure head 2 is born with lower end cover 6 by cavity wall 7, upper end cover 5 with the pressure that lower electrode pressure head 3 produces; And described cavity wall 7, upper end cover 5 immobilize with the volume of the enclosed space that lower end cover 6 is surrounded, and avoid pressure directly to be loaded on powder.
The method of utilizing the auxiliary quick powder preparing device of above-mentioned electric current to prepare powder comprises the steps:
1, opens reaction cavity 1, can place conduction or non-conductive crucible in reaction cavity 1 inside, powder is placed in the crucible;
2, the off-response cavity 1; Keep the enclosed space volume of reaction cavity to immobilize; Directly connect direct current or high-frequency pulse current at top electrode pressure head 2 and lower electrode pressure head 3, electric current produces heat through reaction cavity, provides the powder reaction required thermal environment; Being rapidly heated of realization response cavity 1, heat-up rate is by direct current or the control of high-frequency pulse current size;
Measure the temperature of powder in the reaction cavity 1 through last infrared thermometer, powder heats up according to preset temp, treats that powder reaches required Heating temperature and after this temperature is incubated the corresponding time, and that accomplishes powder adds the hot preparation process;
3, close current is opened reaction cavity, takes out powder.
Above-described embodiment specifies technical scheme of the present invention; Be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All any modifications of in principle scope of the present invention, being made, replenish or similar fashion substitutes etc., all should be included within protection scope of the present invention.
Claims (10)
1. the auxiliary method for preparing powder fast of electric current is characterized in that: adopt the auxiliary quick powder preparing device of electric current to accomplish according to following steps;
The auxiliary quick powder preparing device of described electric current comprises the reaction cavity (1) that is used to place powder, is arranged on reaction cavity (1) two ends, reaction cavity (1) is rapidly heated through input dc power stream or high-frequency pulse current top electrode pressure head (2) and lower electrode pressure head (3), and be positioned at reaction cavity (1) and go up, be used to place the thermometer hole (4) of temperature-measuring part with monitoring reaction cavity (1) temperature; It is characterized in that: described reaction cavity (1) is the enclosed space that is surrounded by cavity wall (7), upper end cover (5) and lower end cover (6); Upper end cover (5) is connected with top electrode pressure head (2); Lower end cover (6) is connected with lower electrode pressure head (3); During working order, top electrode pressure head (2) is born with lower end cover (6) by cavity wall (7), upper end cover (5) with the pressure that lower electrode pressure head (3) produces, and the volume of described enclosed space immobilizes;
Step 1, powder is placed in the reaction cavity (1), keep the enclosed space volume of reaction cavity (1) to immobilize;
Step 2, at top electrode pressure head (2) and lower electrode pressure head (3) turned direct current or high-frequency pulse current; Electric current produces heat through reaction cavity (1); Reaction cavity (1) heats up; Place the powder in the reaction cavity (1) to heat up, heat-up rate is by direct current or the control of high-frequency pulse current size thereupon;
Step 3, measure the temperature in the reaction cavity (1) through temperature-measuring part, treat that powder reaches required Heating temperature and behind this temperature insulation certain hour, that accomplishes powder adds the hot preparation process;
Step 4, close current after question response cavity (1) cooling, are taken out powder.
2. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2, it is characterized in that: in the described step 1, powder is placed in the crucible, and crucible is placed in the reaction cavity (1).
3. the auxiliary method for preparing powder fast of electric current according to claim 1; It is characterized in that: the xsect 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 xsect of a certain position of lower end cover (6) makes lower end cover (6) be buckled in cavity wall (7) bottom greater than reaction cavity (1) diameter.
4. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2; It is characterized in that: described lower end cover (6) is combined as a whole with cavity wall (7); The xsect of a certain position of upper end cover (5) makes upper end cover (5) be buckled in cavity wall (7) top greater than reaction cavity (1) diameter.
5. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2 is characterized in that: described cavity wall (7), upper end cover (5) are processed by the HMP electro-conductive material respectively with lower end cover (6).
6. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2 is characterized in that: described cavity wall (7), upper end cover (5) are processed by graphite material respectively with lower end cover (6).
7. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2, it is characterized in that: described thermometer hole (4) is arranged on upper end cover (5) or lower end cover (6) position.
8. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2, it is characterized in that: described temperature-measuring part is last infrared thermometer.
9. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2, it is characterized in that: the temperature of described reaction cavity (1) is controlled at 400～2200 degrees centigrade, and temperature rise rate is controlled at 1～400 degrees celsius/minute.
10. the auxiliary method for preparing powder fast of electric current according to claim 1 and 2 is characterized in that: the hot preparation process that adds of described powder comprises that the annealing of powder and normalizing thermal treatment, solid-state phase changes, solid state reaction are synthesized, solid and gas two phase reaction synthetic process.
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| CN105333731A (en) * | 2015-11-20 | 2016-02-17 | 燕山大学 | Discharge smelting device and smelting method for ZrTiAlV alloy |
| CN105798297A (en) * | 2016-03-23 | 2016-07-27 | 北京科技大学 | Electric sintering metal material 3D printing device and printing technology thereof |
| 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 |
| CN106116559A (en) * | 2016-08-30 | 2016-11-16 | 西南交通大学 | A kind of electric field-assisted ceramic low-temp quick-combustion device |
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| CN105333731A (en) * | 2015-11-20 | 2016-02-17 | 燕山大学 | Discharge smelting device and smelting method for ZrTiAlV alloy |
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| 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 |
| 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 |
| 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 |
| CN106238732A (en) * | 2016-08-30 | 2016-12-21 | 浙江晨华科技有限公司 | A kind of discharge plasma sintering system |
| CN106116559A (en) * | 2016-08-30 | 2016-11-16 | 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 |
| CN108580902A (en) * | 2018-05-02 | 2018-09-28 | 东北大学 | A kind of electrochemistry adjuvant powders metallurgy prepares POROUS TITANIUM or the method for titanium alloy |
| CN108580902B (en) * | 2018-05-02 | 2019-06-04 | 东北大学 | A kind of method that electrochemistry adjuvant powders metallurgy prepares POROUS TITANIUM or titanium alloy |
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| CN109654888A (en) * | 2019-01-15 | 2019-04-19 | 太原理工大学 | A kind of high-frequency impulse discharge sintering system |
| CN109734445A (en) * | 2019-03-06 | 2019-05-10 | 武汉理工大学 | A kind of electric field-assisted flash sintering method of Ultra-fine Grained hafnium oxide ceramics |
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| CN114349005A (en) * | 2022-01-14 | 2022-04-15 | 天津大学 | Preparation method of high-entropy metal carbide ceramic powder |
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