CN104616880B - A kind of method for producing Sintered NdFeB magnet - Google Patents

A kind of method for producing Sintered NdFeB magnet Download PDF

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CN104616880B
CN104616880B CN201310536214.6A CN201310536214A CN104616880B CN 104616880 B CN104616880 B CN 104616880B CN 201310536214 A CN201310536214 A CN 201310536214A CN 104616880 B CN104616880 B CN 104616880B
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room
agglomerating chamber
vacuum
chamber
temperature
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CN104616880A (en
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王浩颉
张瑾
赵玉刚
陈国安
朱伟
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SANVAC (BEIJING) MAGNETICS CO Ltd
Beijing Zhong Ke San Huan High Tech Co Ltd
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SANVAC (BEIJING) MAGNETICS CO Ltd
Beijing Zhong Ke San Huan High Tech Co Ltd
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Abstract

The present invention provides a kind of method for producing Sintered NdFeB magnet, carries out, comprises the following steps in the continuous fritting furnace for being provided with preparation room, dewaxing room, degassing room, the first agglomerating chamber, the second agglomerating chamber, the 3rd agglomerating chamber and cooling chamber:1) prepare;2) dewax, dewaxing temperature is 300~350 DEG C;3) deaerate;4) it is pre-sintered;5) sinter;6) cool down, wherein dewaxing, deaerating, be pre-sintered equal with sintering step duration.After terminating, first order timeliness is carried out in the 3rd agglomerating chamber, is then cooled down.If blank is inadequate in the sintering time of the second agglomerating chamber, supplement sintering can also be carried out in the 3rd agglomerating chamber.

Description

A kind of method for producing Sintered NdFeB magnet
Technical field
The present invention provides a kind of method for producing Sintered NdFeB magnet, and in particular to one kind is produced using continuous fritting furnace The method of sintered NdFeB.
Background technology
The sintering of Sintered NdFeB magnet is carried out under vacuum condition, high temperature.During using single chamber sintering furnace, sintering process In the material that discharges can reduce the vacuum of sintering furnace, and cause the pollution to sintering furnace, and then influence the quality of product.It is de- The hydrogen that gas process discharges can corrode the joint of the thermocouple end in sintering furnace, cause thermocouple hydrogen embrittlement and be broken, so as to influence Sinter the quality of blank.In addition, during using single chamber sintering furnace, occur to repeat to heat up and cooling, so cause energy loss larger, Produce the cost increase of blank.When long-term use of, the uniformity and uniformity of single chamber sintering furnace in-furnace temperature reduce, so as to influence The uniformity of magnet.
The Chinese utility model patent of Japanese Patent Laid-Open 9-222282 and Application No. 201220584986.8 is distinguished Provide a kind of continuous fritting furnace.Each room of continuous fritting furnace is the space of independent closed, unaffected between each other, each Temperature is relatively stable between room.Because the material transmission between each room of continuous fritting furnace is streamlined mode, the life of each room Production speed needs beat consistent, could rationally reduce energy consumption.
When the temperature for the room that dewaxes is more than 400 DEG C, for the material batch that weight is larger, deflation time can be longer, very It is inconsistent in agglomerating chamber's residence time beat with material so as to cause to the time for exceeding sintering needs, and then be unfavorable for protecting Hold the uniform of sintering in-furnace temperature.When carrying out 850~1080 DEG C of multi-temperature section sintering in an agglomerating chamber, due to sintering Indoor range of temperature is larger, influences the stabilization of sintering stage temperature in continuous production.In addition, in mass production process In, in the high temperature sintering stage, material reaches design temperature from actual temperature and the lag period be present.
In addition, the Chinese utility model patent of Application No. 201220584986.8 further relates to increase a timeliness room.So And blank batch quantity it is big when, terminating rear blank is generally cooled to less than 80 DEG C, and first order aging temp is 800~900 DEG C, reaching this temperature needs more than 1.5h.Second level aging temp is 450~550 DEG C, and this is dropped to after first order completion of prescription One temperature needs more than 2h, also needs to be incubated 2~4h in second level aging temp in addition.So stop of the material in timeliness room Time is more than 6h.This requires to mismatch with residence time of the material in other rooms of continuous oven, causes material to be needed in other rooms Treat that certain time could enter timeliness room.
In addition, in order to improve the coercivity of blank and squareness by the gross, it is necessary in first order aging temp and the second level The quick cooling after terminating of effect temperature.If second level timeliness is carried out in same timeliness room, without first order timeliness Quick cooling procedure afterwards, it is likely that influence the raising of properties of product.
The content of the invention
In view of the above problems, the present invention provides a kind of method for producing Sintered NdFeB magnet, enters in continuous fritting furnace OK, this method can ensure that material is equal in continuous fritting furnace each indoor residence time, and beat is consistent, and pre- due to adding Sintering stage, it is ensured that the stabilization of sintering stage temperature, so as to improve the uniformity of magnet performance.
It is described production Sintered NdFeB magnet method, be provided with preparation room, dewaxing room, degassing room, the first agglomerating chamber, Carry out, comprise the following steps in the continuous fritting furnace of second agglomerating chamber, the 3rd agglomerating chamber and cooling chamber:
1) prepare
When the vacuum of preparation room is higher than 2300Pa, start auto-programming, when vacuum is higher than 40Pa, to preparation room Inert gas or compressed air are filled with, material enters the preparation room, when vacuum is higher than 30Pa, from the preparation room to de- Wax room conveys the material;
2) dewax
After the material enters the dewaxing room, when vacuum is higher than 600Pa, heat temperature raising 0.5 hour, temperature reaches 300~350 DEG C, insulation;It is incubated after terminating when vacuum is higher than 70Pa, the thing is conveyed from the dewaxing room to degassing room Material;
3) deaerate
After the material enters the degassing room, when vacuum is higher than 700Pa, heat up 0.5 hour, temperature reaches 700 ~820 DEG C, insulation, it is incubated after terminating when vacuum is higher than 30Pa, the thing is conveyed to the first agglomerating chamber from the degassing room Material;
4) it is pre-sintered
After the material enters first agglomerating chamber, when vacuum is higher than 60Pa, heat up 5~10min, and temperature reaches 700~820 DEG C, 1h~1h55min is incubated, then is heated up 0.5 hour, now temperature is lower than sintering temperature 10~20 DEG C, is incubated, and protects Temperature terminate after when vacuum is higher than 10Pa, the material is conveyed from first agglomerating chamber to the second agglomerating chamber;
5) sinter
After the material enters second agglomerating chamber, when vacuum is higher than 60Pa, heat up 10 minutes, temperature reaches burning Junction temperature, insulation;
6) cool down
After the material is transported into the cooling chamber, when vacuum is higher than 20Pa, indifferent gas is filled with to cooling chamber Body, then being cooled down, cool time is 2~3 hours, and when vacuum is higher than 10Pa, material is come out of the stove,
Wherein, dewax, deaerate, be pre-sintered equal with sintering step duration.
Preferably, the step of method of the production Sintered NdFeB magnet also includes first order timeliness, the described 3rd Agglomerating chamber is carried out, and the material is after second agglomerating chamber delivers into the 3rd agglomerating chamber, when the 3rd agglomerating chamber Vacuum when being higher than 60Pa, vacuum cool-down 2 hours, then heat up 0.5 hour, temperature reaches 800~950 DEG C, insulation.
Preferably, the step of method of the production Sintered NdFeB magnet also includes supplement sintering, burnt the described 3rd Knot is carried out in room, after the material delivers into three agglomerating chamber from second agglomerating chamber, the 3rd agglomerating chamber Heat up 10min, after temperature reaches the sintering temperature, insulation.
Brief description of the drawings
Fig. 1 is the organigram of seven Room continuous vacuum sintering furnaces used in embodiment.
Fig. 2 is the method flow diagram that Sintered NdFeB magnet is produced in embodiment.
Embodiment
The technical scheme of the specific embodiment of the invention is illustrated below in conjunction with accompanying drawing.
In the present embodiment, sintering furnace used is seven Room continuous vacuum sintering furnaces (hereinafter referred to as sintering furnace), and it is constructed As shown in figure 1, it is provided with prep stand 5, preparation room 8, dewaxing room 9, degassing room 10, the first agglomerating chamber 11, the second agglomerating chamber 12, the Three agglomerating chamber 13, cooling chamber 14 and taking-out platform 15.
Blank material is piled up on prep stand 5.Dewaxing room 9 is provided with the dewaxing crucible 2 for being dewaxed to blank material, takes off Heater is provided between wax room 9 and dewaxing crucible 2, is furnished with refrigerating plant 3 on the crucible 2 that dewaxes.Preparation room 8, dewaxing room 9, degassing room 10th, the first agglomerating chamber 11, the second agglomerating chamber 12, the 3rd agglomerating chamber 13 and cooling chamber 14 are both provided with mechanical pump and lobe pump vacuum System, the first agglomerating chamber 11 and the second agglomerating chamber 12 are additionally provided with diffusion pump, and diffusion pump is connected with refrigerating plant 3 and expanded to cool down Dissipate the oil vapour of pump.Cooling chamber 14 is provided with continuous frequency conversion formula air blower 4 and is used to cool down material.Pass through lock between two neighboring room Plate valve 7 is spaced apart, and material is conveyed by roller 6 between two neighboring room.
The method for producing Sintered NdFeB magnet is illustrated below.
The weight of each batch blank to be sintered is 200~350kg.
Blank to be sintered is in dewaxing room 9, degassing room 10, the first agglomerating chamber 11, the second agglomerating chamber 12 and the 3rd agglomerating chamber 13 Residence time is equal, and this time is set as that pitch time (Takt time) T, pitch time T is 3~5h, can so protect It is consistent to hold the rhythm that blank material circulates along each room.
To preparation room 8, dewaxing room 9, degassing room 10, the first agglomerating chamber 11, the second agglomerating chamber 12, the 3rd agglomerating chamber 13 and cold But each in room 14, SET1, SET2 and SET3 value are set respectively.SET1 represents the minimum vacuum alarming value of each room, When vacuum is less than SET1 values, do not start auto-programming, the body of heater of corresponding each room does not heat, while alarm.SET2 Represent that each room body of heater performs the minimum vacuum degree of automatic heating, i.e., when vacuum is higher than SET2 values, the stove of corresponding each room Body starts to perform automatic heating, otherwise continues to vacuumize until vacuum is higher than SET2 values.SET3 is represented between adjacent two Room Slide valve automatically turns on required minimum vacuum angle value.It should be noted that the SET2 values of preparation room 8 are represented when vacuum is high When SET2 values, automatically begin to be filled with inert gas or compressed air into preparation room 8, and the SET2 values of cooling chamber 14 are to represent When vacuum is higher than SET2, automatically begin to be filled with inert gas into cooling chamber 14, air blower is actuated for after inflation Cooling.
The parameter setting of each room is as shown in table 1 above.
Table 1
Above-mentioned SET1, SET2 and SET3 value is the minimum of technological requirement, and the vacuum higher than above-mentioned value is suitable for even Continuous vacuum sintering furnace is produced, if vacuum is less than above-mentioned value, blank has the risk of oxidation.
Specific sintering process is as follows.
The first step, the preparation that sintering furnace enters before automatic running.Vacuumize, when the vacuum of preparation room 8 is higher than During 2300Pa, auto-programming is run.When the vacuum of preparation room 8 is higher than 40Pa, inert gas or compression are filled with to preparation room 8 Air, material is then conveyed into preparation room, closes slide valve 7.When vacuum is higher than 30Pa, preparation room 8 and dewaxing are opened Slide valve between room 9, material is conveyed from preparation room 8 to dewaxing room 9.
Second step, dewaxing.After material enters dewaxing room 9, slide valve is closed.Then vacuumize, when vacuum is higher than 600Pa When, heating is begun to warm up, heat up 0.5h, and temperature reaches 300~350 DEG C, insulation.When vacuum is higher than 70Pa, dewaxing room 9 with Slide valve 3 between degassing room 10 is opened, and material is conveyed from dewaxing room 9 to degassing room 10.
3rd step, degassing.After material enters degassing room 10, slide valve is closed, then begins to warm up heating, heating-up time 0.5h, temperature rise to 700~820 DEG C, insulation.At this point it is possible to start to convey the thing of next batch from preparation room 8 to dewaxing room 9 Material.After insulation terminates, if vacuum is higher than 30Pa, the slide valve between the degassing agglomerating chamber 11 of room 10 and first is opened, from Degassing room 10 conveys material to the first agglomerating chamber 11.
4th step, it is pre-sintered.After material enters the first agglomerating chamber 11, slide valve is closed.When vacuum is higher than 60Pa, open Beginning heats to the first agglomerating chamber 11, and heat up 5~10min, and temperature rises to 700~820 DEG C, is incubated 1h~1h55min.Continue to add Heat, heat up 0.5h, when temperature reaches 10~20 DEG C lower than sintering temperature, insulation.After insulation terminates, when vacuum is higher than 10Pa When, the slide valve between the first agglomerating chamber 11 and the second agglomerating chamber 12 is opened, it is defeated from the first agglomerating chamber 11 to the second agglomerating chamber 12 Send material.
5th step, sintering.After material enters the second agglomerating chamber 12, slide valve is closed.Then heat temperature raising, heat up 10min, Temperature rises to the temperature (that is, sintering temperature) needed for sintering, insulation.Formula, melting steel ingot of the sintering temperature according to slug press Technique, crushing process, milling granularity and the difference of blank control oxygen amount are adjusted, and temperature range is 1040~1100 DEG C.Therefore Need, according to different sintering temperatures, to set different sintering temperature curves, be input in the control program of sintering furnace, to meet not With the sintering of blank.When vacuum is higher than 10Pa, the slide valve between the second agglomerating chamber 12 and the 3rd agglomerating chamber 13 is opened, from Second agglomerating chamber 12 conveys material to the 3rd agglomerating chamber 13.
6th step, first order timeliness, carried out in the 3rd agglomerating chamber 13.After material enters the 3rd agglomerating chamber 13, flashboard is closed Valve.Then vacuum cool-down 2h, next heat up 0.5h, and temperature reaches 800~950 DEG C, is then incubated.When vacuum is higher than 30Pa When, the slide valve between the 3rd agglomerating chamber 13 and cooling chamber 14 is opened, material is conveyed from the 3rd agglomerating chamber 13 to cooling chamber 14.
7th step, cooling.After material enters cooling chamber 14, slide valve is closed.When vacuum is higher than 20Pa, to cooling chamber 14 are filled with inert gas, and inflation terminates rear air blower and is actuated for cooling down, and cools down 2~3h.When vacuum is higher than 10Pa, open The slide valve of cooling chamber 14, material is come out of the stove, and blank tapping temperature is less than 60 DEG C.
The second level timeliness of blank is to be carried out after cooling is come out of the stove in independent one-way fired furnace, so that one-way fired furnace exists for a long time One low-temperature zone operation, it is ensured that the material of different batches carries out the uniform uniformity of temperature during the timeliness of the second level, so as to protect Holding the magnetic property of product has good uniformity, and can extend the service life of one-way fired furnace.
Timeliness room of 3rd agglomerating chamber 13 as first order aging temp, can save the heating-up time, reduce energy consumption.
In addition, the 3rd agglomerating chamber 13 can be also used for supplement sintering, further closely knit sintering is carried out to blank.Second After the sintering of agglomerating chamber 12 terminates, if blank is not up to required density, supplement burning can be carried out in the 3rd agglomerating chamber 13 Knot, temperature is identical with foregoing sintering temperature, and heating 10min, soaking time is increased according to being actually needed, but the increased time To be less than pitch time T.Insulation terminate after, carry out vacuum cool-down automatically, then by material deliver into cooling chamber 14 carry out it is fast Quickly cooling is but.
, can be by under when the material in preparation room 8 enters in dewaxing room 9 in the case of multiple batch continuous productions A batch of material is positioned ready for carrying out pan feeding preparation on platform, but the pan feeding time interval maximum of front and rear two batches is no more than 2 times of pitch time T, the i.e. latest time of pan feeding are that the previous batches in the room 9 that dewaxes enter before degassing room 10.
If the dewaxing temperature of room 9 is set in more than 400 DEG C, it will causes the deflation in dewaxing process violent, in 3~5h Vacuum is difficult to reach required condition of high vacuum degree, so as to cause material long in the dewaxing residence time of room 9, influences production procedure Beat.And the above method is by rationally controlling the temperature and SET2, SET3 value of dewaxing, it is ensured that the beat system of whole flow process One, while also ensure that the performance of sintering blank.Moreover, material fixes consistent, flow beat production in each room residence time, Save energy consumption and improve the efficiency and uniformity of blank production.
According to the above method, each indoor temperature change is small, relatively stable.In addition, added in the first agglomerating chamber 11 Pre-sintered state, it is existing between the actual temperature of blank material and the sintering temperature of setting during so as to compensate for mass production Lag period so that into the blank to be sintered in the second agglomerating chamber 12 actual temperature differ with the furnace temperature of the second agglomerating chamber 12 compared with It is small, be so advantageous to blank and sinter uniform consistent.
Embodiment 1
Pitch time T is set as 3h.
Raw material are prepared by the formula that single batch weight is 200k g, pre- performance is N44H, raw material pass through belt-rejecting technology Thin slice steel ingot is made, HD process is crushed, and airflow milling milling, blank is formed by orientation compacting under inert gas shielding Crude green body, blank crude green body is put into magazine, is filled with inert gas and carries out sealing protection.
Next, blank is sintered.
First, the parameter of each room of sintering furnace is set, it is specific as shown in table 2.
Table 2
First, sintering furnace is started, into the preparation of automatic running, the vacuum system of each room vacuumizes, vacuum Reach SET3 requirement and enter automatic running state after meeting other automatic running conditions.
Next, the magazine (hereinafter referred to as material) equipped with blank is positioned ready on platform, the program of automatic running is performed. Now N is filled with into preparation room 82, after being balanced with ambient pressure, slide valve between prep stand and preparation room 8 is opened, material by Roller is transported to preparation room 8, is then shut off slide valve, vacuumizes, and when vacuum is higher than SET3 values (30Pa), opens preparation room Slide valve between 8 and dewaxing room 9, material is conveyed from preparation room 8 to dewaxing room 9.
After material enters dewaxing room 9, slide valve is closed.Then vacuumize, vacuum starts to add when being higher than SET2 (600Pa) Heat heating, heat up 0.5h, then temperature is incubated 2.5h up to 300 DEG C.Thus complete the dewaxing to blank.When in dewaxing room 9 Vacuum reaches 15Pa, i.e., higher than SET3 values (30Pa) when, open dewaxing room 9 and deaerate room 10 between slide valve 3, from dewaxing Room 9 conveys material to degassing room 10.
After material enters degassing room 10, slide valve is closed.Then begin to warm up heating, heat up 0.5h, temperature up to 700 DEG C, Next insulation 2.5h.At this point it is possible to start to convey the blank material of second lot from preparation room 8 to dewaxing room 9.Material is de- After air chamber 10 is incubated 2.5h, the vacuum of degassing room 10 be 10Pa, i.e., higher than SET3 values (30Pa) when, opening deaerates room 10 and the Slide valve between one agglomerating chamber 11, material is conveyed from degassing room 10 to the first agglomerating chamber 11.
After material enters the first agglomerating chamber 11, slide valve is closed.Then heating is begun to warm up, heat up 5min, and temperature reaches 700 DEG C, it is incubated 1h.Followed by pre-sintering, heat temperature raising 0.5h, temperature reaches 1040 DEG C (10 DEG C lower than sintering temperature), protects Warm 1.5h.After said procedure terminates, the vacuum of the first agglomerating chamber 11 reaches 1Pa, i.e., higher than SET3 values (30Pa) when, open the Slide valve between one agglomerating chamber 11 and the second agglomerating chamber 12, material is conveyed from the first agglomerating chamber 11 to the second agglomerating chamber 12.
After material enters the second agglomerating chamber 12, slide valve is closed.Crucial high temperature is carried out to blank in the second agglomerating chamber 12 Sintering, heat temperature raising 10min, temperature reach 1050 DEG C, are then incubated 2h50min.Insulation terminate after, the second agglomerating chamber 12 it is true Reciprocal of duty cycle reaches 5X10-3Pa, i.e., higher than SET3 values (30Pa), now open the lock between the second agglomerating chamber 12 and the 3rd agglomerating chamber 13 Plate valve, material is conveyed from the second agglomerating chamber 12 to the 3rd agglomerating chamber 13.
After material enters the 3rd agglomerating chamber 13, slide valve is closed.3rd agglomerating chamber 13 is used as the first aging temp room.It is first First, to the vacuum cool-down 2h of the 3rd agglomerating chamber 13, then heat up 0.5h, and temperature reaches 800 DEG C, is then incubated 0.5h.Insulation terminates The 3rd agglomerating chamber 13 and the slide valve of cooling chamber 14 are opened afterwards, and material is conveyed from the 3rd agglomerating chamber 13 to cooling chamber 14.
Come out of the stove after cooling chamber 14, cooling material 2h.
In whole sintering process, material is in dewaxing room 9, degassing room 10, the first agglomerating chamber 11, the second agglomerating chamber 12 and the Residence time in three agglomerating chamber 13 is all 3h.Whole sintering process is smooth, alarm of not breaking down.After material is come out of the stove, inspection The outward appearance for looking into blank does not find to aoxidize.The density of blank in all magazines is inspected by random samples, is as a result 7.58~7.61g/ cm3, show that the uniformity for sintering blank is good.
Embodiment 2
Pitch time T is set as 4h.
Raw material are prepared by the formula that single batch weight is 300kg, pre- performance is N45SH, raw material pass through belt-rejecting technology Thin slice steel ingot is made, HD process crushes, airflow milling milling, and it is thick by orientation compacting to form blank under inert gas shielding Base, blank crude green body is then put into magazine, is filled with inert gas seal protection.
Next, blank is sintered.
First, the parameter of each room of sintering furnace is set, it is specific as shown in table 3.
Table 3
Sintering process is same as Example 1.
In whole implementation process, material is in dewaxing room 9, degassing room 10, the first agglomerating chamber 11, the second agglomerating chamber 12 and the Residence time in three agglomerating chamber 13 is all 4h, and whole sintering process is smooth, alarm of not breaking down.Material checks after coming out of the stove Outward appearance is not found to aoxidize, and the density of the material in all magazines is inspected by random samples, and Examined is 7.59~7.61g/cm3, Show that the blank uniformity of sintering is good.
Embodiment 3
Pitch time T is set as 5h.
Raw material are prepared by the formula that single batch weight is 350kg, pre- performance is N45SH, raw material pass through belt-rejecting technology Thin slice steel ingot is made, HD process is crushed, and airflow milling milling, blank is formed by orientation compacting under inert gas shielding Crude green body, blank crude green body is put into magazine, is filled with inert gas seal protection.
Next, blank is sintered.
First, the parameter of each room of sintering furnace is set, it is specific as shown in table 4.
Table 4
Sintering process is same as Example 1.
In whole implementation process, material is in dewaxing room 9, degassing room 10, the first agglomerating chamber 11, the second agglomerating chamber 12 and the Residence time in three agglomerating chamber 13 is all 5h, and whole sintering process is smooth, alarm of not breaking down.Material checks after coming out of the stove Outward appearance does not find to aoxidize.The density of material in all magazines is inspected by random samples, Examined is 7.59~7.61g/cm3, Show that the uniformity for sintering blank is good.
Embodiment 4
Pitch time T is set as 4h.
Raw material are prepared by the formula that single batch weight is 300kg, pre- performance is N48H, raw material pass through belt-rejecting technology system Thin slice steel ingot is obtained, HD process is crushed, and airflow milling milling, is put under inert gas shielding by orientation slug press crude green body Enter magazine, and be filled with inert gas seal protection.
Next, blank is sintered.
First, the parameter of each room of sintering furnace is set, it is specific as shown in table 5.
Table 5
In the present embodiment, in addition to carrying out supplement sintering in the 3rd agglomerating chamber 13, other steps and the phase of embodiment 1 Together.
In whole implementation process, material is in dewaxing room 9, degassing room 10, the first agglomerating chamber 11 and the second agglomerating chamber 12 Residence time is all 4h, and whole sintering process is smooth, alarm of not breaking down.Material, which is come out of the stove, checks that outward appearance does not find oxygen Change.The density of material in all magazines is inspected by random samples, Examined is 7.54~7.57g/cm3, show that sintering furnace sinters The uniformity of blank is good.
Be described in detail technical scheme above in association with embodiment and embodiment, but the present invention not by It is limited to this.On the premise of the object of the invention is realized, those skilled in the art can make various changes and deformation to the present invention.

Claims (3)

1. a kind of method for producing Sintered NdFeB magnet, preparation room, dewaxing room, degassing room, the first agglomerating chamber, the are being provided with Carry out, comprise the following steps in the continuous fritting furnace of two agglomerating chamber, the 3rd agglomerating chamber and cooling chamber:
1) prepare
When the vacuum of preparation room is higher than 40Pa, inert gas or compressed air are filled with, material enters the preparation room, takes seriously When reciprocal of duty cycle is higher than 30Pa, the material is conveyed from the preparation room to the dewaxing room;
2) dewax
After the material enters the dewaxing room, when vacuum is higher than 600Pa, heat temperature raising 0.5 hour, temperature reaches 300 ~350 DEG C, insulation, it is incubated after terminating when vacuum is higher than 70Pa, the thing is conveyed from the dewaxing room to the degassing room Material;
3) deaerate
After the material enters the degassing room, when vacuum is higher than 700Pa, heat up 0.5 hour, temperature reaches 700~820 DEG C, insulation, it is incubated after terminating when vacuum is higher than 30Pa, the thing is conveyed to first agglomerating chamber from the degassing room Material;
4) it is pre-sintered
After the material enters first agglomerating chamber, when vacuum is higher than 60Pa, heat up 5~10min, and temperature reaches 700 ~820 DEG C, 1h~1h55min is incubated, then is heated up 0.5 hour, now temperature lower than the sintering temperature that the second agglomerating chamber sets 10 ~20 DEG C, insulation, it is incubated after terminating when vacuum is higher than 10Pa, is conveyed from first agglomerating chamber to second agglomerating chamber The material;
5) sinter
After the material enters second agglomerating chamber, when vacuum is higher than 60Pa, heat up 10 minutes, temperature reaches the burning Junction temperature, insulation;
6) cool down
After the material is transported into the cooling chamber, when vacuum is higher than 20Pa, inert gas is filled with to cooling chamber, so After cooled down, cool time be 2~3 hours, when vacuum is higher than 10Pa, the material is come out of the stove,
Wherein, dewax, deaerate, be pre-sintered equal with sintering step duration.
2. the method for production Sintered NdFeB magnet according to claim 1, it is characterised in that also including first order timeliness The step of, the 3rd agglomerating chamber carry out, the material after second agglomerating chamber delivers into the 3rd agglomerating chamber, When the vacuum of the 3rd agglomerating chamber is higher than 60Pa, vacuum cool-down 2 hours, then heat up 0.5 hour, temperature reaches 800 ~950 DEG C, insulation.
3. the method for production Sintered NdFeB magnet according to claim 1, it is characterised in that also include supplement sintering Step, carried out in the 3rd agglomerating chamber, when the material delivers into the 3rd agglomerating chamber from second agglomerating chamber Afterwards, heat up 10min, after temperature reaches the sintering temperature, insulation.
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CN106802078B (en) * 2017-01-03 2019-03-29 新冶高科技集团有限公司 A kind of neodymium iron boron high vacuum pressure sintering furnace
CN108376607A (en) * 2017-12-31 2018-08-07 江西荧光磁业有限公司 A kind of preparation method reducing heavy rare earth sintered NdFeB
CN108637249A (en) * 2018-06-06 2018-10-12 山西大缙华磁性材料有限公司 A kind of neodymium iron boron magnetic body sintering process
CN110534278A (en) * 2019-08-15 2019-12-03 宁波爱维森材料研发科技有限公司 A kind of sintering method of sintered Nd-Fe-B permanent magnetic material
CN117146580B (en) * 2023-11-01 2023-12-29 沈阳广泰真空科技股份有限公司 Eight-chamber vacuum continuous sintering furnace control method and eight-chamber vacuum continuous sintering furnace

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