CN102390079A - High-pressure sintering combined die and high-pressure rapid sintering method for preparing nanometer ceramic thereof - Google Patents
High-pressure sintering combined die and high-pressure rapid sintering method for preparing nanometer ceramic thereof Download PDFInfo
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- CN102390079A CN102390079A CN2011102878591A CN201110287859A CN102390079A CN 102390079 A CN102390079 A CN 102390079A CN 2011102878591 A CN2011102878591 A CN 2011102878591A CN 201110287859 A CN201110287859 A CN 201110287859A CN 102390079 A CN102390079 A CN 102390079A
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Abstract
The invention discloses a high-pressure sintering combined die, which comprises a hollow cylindrical outer die, a hollow cylindrical inner die, one pair of cylindrical inner pressure heads, one pair of cylindrical metallic laminations, one pair of cylindrical ceramic laminations and one pair of cylindrical outer pressure heads, wherein the side face of the outer die is provided with a through hole into which a thermocouple is inserted; the hollow cylindrical inner die is arranged in the hollow cavity body of the outer die; the side face of the inner die is provided with a blind hole into which the thermocouple is inserted; the outer die and the inner die are in close fit, and the centre line of the through hole into which the thermocouple is inserted on the side face of the outer die and the centre line of the blind hole into which the thermocouple is inserted on the side face of the inner die coincide; the cylindrical inner pressure heads are half inserted into the upper end and the lower end of the hollow cavity body of the inner die; the inserted inner pressure heads and the hollow cavity body of the inner die form a die cavity; the cylindrical metallic laminations are arranged outside the inner pressure heads; the cylindrical ceramic laminations are arranged outside the cylindrical metallic laminations; the cylindrical outer pressure heads are arranged outside the cylindrical ceramic laminations; and the ceramic laminations and the outer pressure heads are in the close fit with the outer die. The invention also discloses a high-pressure rapid sintering method for preparing a nanometer ceramic by adopting the die. By adopting the die and the sintering method disclosed by the invention, the rapid low-temperature compact sintering can be realized on a nanometer ceramic material.
Description
Technical field
The present invention relates to the Fast Sintering technical field of ceramic material, be specifically related to the high pressure flash sintering method of a kind of high-pressure sinter mould and preparation nano ceramics thereof.
Background technology
Pottery or metal dust pressure sintering mould are owing to generally to its common requirement at aspects such as mechanical behavior under high temperature and thermal conductivity, generally only adopt high-performance graphite or refractory metal material to process.Obviously, under certain sintering temperature, only adopt graphite or refractory metal material obviously can't bear the hundreds of MPa even surpass high pressure or the ultra-high pressure sintering more than the 1GPa.
About sintering mold, all non-pressurised or high-pressure sinter mould of sintering mold in ZL200920034468.7 " a kind of constraint presintering mould of the TiAl of preparation base alloy " and 201110040207.8 " a kind of constraint sintering molds of controlling powder metallurgy blank sintering deformation defect "; And Chinese patent ZL201020211803.9 " a kind of powder metallurgy brake lining pressure sintering mould " just is directed against powder metallurgy brake lining pressure sintering mould, but not the high-pressure sinter mould.Put it briefly, existing sintering mold all can not bear high pressure.
Sintering technology about the nano block pottery; Mainly comprise two-step sintering method, plasma agglomeration (comprising discharge plasma sintering and plasma activated sintering), hot pressed sintering, ultra-high pressure sintering, phase transformation sintering, add sintering aid method etc., wherein plasma agglomeration and ultra-high pressure sintering are respectively typical Fast Sintering and low-temperature sintering technology.In a word, the sintering technology of existing preparation nano block pottery can not be realized not only low temperature but also densification sintering fast simultaneously.
Summary of the invention
In order to overcome the shortcoming that above-mentioned prior art exists; The object of the present invention is to provide the high pressure flash sintering method of a kind of high-pressure sinter mould and preparation nano ceramics thereof; Adopt high-pressure sinter mould of the present invention and sintering method thereof, can realize the low temperature of nano ceramic material and densification sintering fast.
In order to achieve the above object, the technical scheme that the present invention adopted is:
A kind of high-pressure sinter assembling die; The assembled state of this mould does; The external mold 1 that comprises the hollow circular cylinder shape, the side of said external mold 1 are provided with the through hole 8 that thermocouple inserts, and are arranged on the internal mold 5 of the hollow circular cylinder shape in external mold 1 hollow cavity; The side of internal mold 5 is provided with the blind hole 9 that thermocouple inserts; Said external mold 1 is tight fit with internal mold 5 and makes the thermocouple of external mold 1 side insert the central lines of the thermocouple insertion blind hole 9 of through hole 8 and internal mold 5 sides that partly insert the internal mold 5 hollow cavities inner ram 6 of a pair of cylindrical shape at two ends up and down, the rounded face in the said a pair of inner ram 6 insertion internal molds 5 and the hollow cavity of internal mold 5 form die cavity 7; Be arranged on the metallic laminations 4 of a pair of cylindrical shape outside a pair of inner ram 6; Be arranged on the ceramic lamination 3 of the cylindrical shape outside the pair of metal lamination 4, be arranged on the outer ram 2 of the cylindrical shape outside a pair of ceramic lamination 3, said ceramic lamination 3 and outer ram 2 and external mold 1 tight fit.
The thermocouple that said external mold 1 side is provided with inserts through hole 8 and is positioned at middle position up and down, side.
The thermocouple that said internal mold 5 sides are provided with inserts blind hole 9 and is positioned at middle position up and down, side.
Said outer ram 2 is 4: 1～36: 1 with the ratio of the sectional area of inner ram 6.
Said external mold 1, internal mold 5 and outer ram 2 materials are graphite, and metallic laminations 4 materials are supertherm, and ceramic lamination 3 is a silicon carbide ceramics with inner ram 6 materials.
Said supertherm be temperature resistant grade be more than 1000 ℃ Ni base, Co is basic, Nb is basic or the basic alloy of Ti.
Said silicon carbide ceramics is for adopting AlN and Lu
2O
3The silicon carbide ceramics that forms for the pressure sintering of sintering aid.
A kind of high pressure flash sintering method for preparing nano ceramics comprises the steps:
Step 1: nano ceramic powder is packed in the die cavity 7 of the said high-pressure sinter assembling die of claim 1, then the high-pressure sinter assembling die is assembled;
Step 2: the high-pressure sinter assembling die that nano ceramic powder will be housed places the plasma agglomeration stove to carry out sintering: rate of heat addition 100-300 ℃/min; Sintering pressure 100-1000MPa; Sintering temperature 500-800 ℃; Sintered heat insulating time 3-10min, insulation finishes the back pressure relief, is cooled to room temperature with the plasma agglomeration stove and gets final product.
The average grain diameter of the described nano ceramic powder of step 1 is smaller or equal to 50nm.
Compared with prior art; The invention has the beneficial effects as follows: in the plasma agglomeration process; Carry out power and electric transmission through ceramic lamination and metallic laminations between inside and outside two pressure heads of assembling die; And realize high pressure through the cross section product moment of interior outer ram, thereby can realize ceramic material or powdered metallurgical material in short-term, the densification sintering of low temperature and high pressure, be particularly suitable for the low temperature Fast Sintering of block nanometer pottery.
Description of drawings
Fig. 1 is a high-pressure sinter assembling die assembled state vertical view of the present invention.
Fig. 2 be high-pressure sinter assembling die assembled state vertical view of the present invention along A-A to profile.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is done more detailed explanation.
Like Fig. 1, shown in Figure 2; A kind of high-pressure sinter assembling die; The assembled state of this mould does, comprises the external mold 1 of hollow circular cylinder shape, and the side of external mold 1 middle position up and down is provided with the through hole 8 that thermocouple inserts; Be arranged on the internal mold 5 of the hollow circular cylinder shape in external mold 1 hollow cavity; The side of internal mold 5 up and down middle position is provided with blind hole 9 external molds 1 that thermocouple inserts and internal mold 5 for tight fit and the thermocouple that makes the thermocouple of external mold 1 side insert through hole 8 and internal mold 5 sides insert the central lines of blind hole 9, partly inserts the internal mold 5 hollow cavities inner ram 6 of a pair of cylindrical shape at two ends up and down, and a pair of inner ram 6 inserts rounded face and the hollow cavity formation die cavity 7 of internal mold 5 in the internal molds 5; Be arranged on the metallic laminations 4 of a pair of cylindrical shape outside a pair of inner ram 6; Be arranged on the ceramic lamination 3 of the cylindrical shape outside the pair of metal lamination 4, be arranged on the outer ram 2 of the cylindrical shape outside a pair of ceramic lamination 3, said ceramic lamination 3 and outer ram 2 and external mold 1 tight fit.Combination of high pressure sintering mold dimensions of the outer mold 1:
The dimensions of the inner mold 5:
external pressure head 2 size:
The dimensions of the metal laminations 4:
The size of the ceramic laminate 3:
internal dimensions of the indenter 6 :
During use; The high-pressure sinter assembling die is assembled; Assemble method is: as shown in Figure 1, internal mold 5 is inserted in the external mold 1, and the thermocouple that makes the thermocouple of external mold 1 side insert through hole 8 and internal mold 5 sides inserts the central lines of blind hole 9; Second inserts hollow cavity from internal mold 5 hollow cavities will to descend sheet inner ram 6 then; Pack the nano ceramic powder of predetermined amount down that the hollow cavity of sheet inner ram 6 and internal mold 5 forms in the die cavity 7 subsequently into, the last slice inner ram 6 of packing into subsequently is pressed in pair of metal lamination 4 on a pair of inner ram 6 subsequently between two parties; Be inserted in a pair of ceramic lamination 3 in the external mold 1 subsequently and be pressed on the pair of metal lamination 4, be inserted in outer ram 2 in the external mold 1 at last and be pressed on a pair of ceramic lamination 3.
Embodiment one
(1) pre-prepared of high-pressure sinter assembling die
(1) The Shanghai Toyo Tanso Co., Ltd. provides high-performance graphite material into the thermocouple inserted into the through hole has a size of:
The outer mold 1, size:
5 and the inner mold size:
external pressure head 2; would Model GH3030 Ni-base superalloy processed into a size:
metal laminations 4.
(2) adopt the plasma activated sintering method with ball mill mixing after the quality proportioning be 80: 15: 5 SiC, AlN and Lu
2O
3Powder sinters under the sintering condition of 300 ℃/min of heating rate, 1600 ℃ of sintering temperatures, sintering pressure 40MPa, sintered heat insulating time 5min and vacuum 12Pa respectively and is of a size of:
With
Disk, be used separately as ceramic lamination 3 and inner ram 6 after the processing through polishing again.
(2) the high pressure flash sintering method of nano ceramics
The average grain diameter of (1) the German Evonik Degussa company of 0.5g being produced is the P25 nano-TiO of 20～30nm
2Ceramic powders (contains mass ratio and is 20% rutile phase TiO
2With 80% anatase TiO mutually
2) in the die cavity shown in Figure 17 of packing into, and by the high-pressure sinter assembling die that assembles shown in Figure 1.
(2) with the above-mentioned nano-TiO that is equipped with
2The high-pressure sinter assembling die of ceramic powders places plasma activated sintering (PAS) stove to carry out sintering: 500 ℃ of 100 ℃/min of the rate of heat addition, sintering pressure 1000MPa, sintering temperature; Sintered heat insulating time 10min; Treat that insulation finishes the back pressure relief; Be cooled to room temperature with the plasma activated sintering stove, can obtain the block TiO of ceramic crystalline grain average grain diameter less than 100nm
2Pottery.
Embodiment two
(1) pre-prepared of high-pressure sinter assembling die
(1) The Shanghai Toyo Tanso Co., Ltd. provides high-performance graphite material into the thermocouple inserted into the through hole has a size of:
The outer mold 1, size:
5 and the inner mold size:
external pressure head 2; would Model GH3030 Ni-base superalloy processed into a size:
metal laminations 4.
(2) employing hot-pressing sintering method (equipment adopts High-Multi-5000 type multifunctional furnace) is 80: 15: 5 SiC, AlN and Lu with quality proportioning behind the ball mill mixing
2O
3Powder is to sinter under 40MPa and the nitrogen atmosphere to be of a size of at 1850 ℃ of sintering temperatures, temperature retention time 60min, pressure respectively:
With
Disk, be used separately as ceramic lamination 3 and inner ram 6 after the processing through polishing again.
(2) the high pressure flash sintering method of nano ceramics
The average grain diameter of (1) the German Evonik Degussa company of 0.5g being produced is the P25 nano-TiO of 20～30nm
2Ceramic powders (contains mass ratio and is 20% rutile phase TiO
2With 80% anatase TiO mutually
2) in the die cavity shown in Figure 17 of packing into, and by the high-pressure sinter assembling die that assembles shown in Figure 1.
(2) with the above-mentioned nano-TiO that is equipped with
2The high-pressure sinter assembling die of ceramic powders places plasma activated sintering (PAS) stove to carry out sintering: 600 ℃ of 300 ℃/min of the rate of heat addition, sintering pressure 500MP, sintering temperature; Sintered heat insulating time 5min; Treat that insulation finishes the back pressure relief; The plasma activated sintering stove is cooled to room temperature, can obtain the block TiO of ceramic crystalline grain average grain diameter less than 100nm
2Pottery.
Embodiment three
(1) pre-prepared of high-pressure sinter assembling die
(1) The Shanghai Toyo Tanso Co., Ltd. provides high-performance graphite material into the thermocouple inserted into the through hole has a size of:
The outer mold 1, size:
5 and the inner mold size:
external pressure head 2; would Model ECY768 Co-based superalloy processed into a size:
metal laminations 4.
(2) adopt discharge plasma sintering (SPS) method with ball mill mixing after the quality proportioning be 80: 15: 5 SiC, AlN and Lu
2O
3Powder sinters under the sintering condition of 300 ℃/min of heating rate, 1600 ℃ of sintering temperatures, sintering pressure 40MPa, sintered heat insulating time 5min and vacuum 12Pa respectively and is of a size of:
With
Disk, be used separately as ceramic lamination 3 and inner ram 6 after the processing through polishing again.
(2) the high pressure flash sintering method of nano ceramics
(1) with 0.5g Hangzhou ten thousand scape new material Co., Ltds produce, average grain diameter is that 20～30nm and purity >=99.9% nano-MgO ceramic powders are packed in the die cavity shown in Figure 17, and by the high-pressure sinter assembling die that assembles shown in Figure 1.
(2) place discharge plasma sintering (SPS) stove to carry out sintering the above-mentioned high-pressure sinter assembling die that the nano-MgO ceramic powders is housed: 800 ℃ of 200 ℃/min of the rate of heat addition, sintering pressure 200MPa, sintering temperature; Sintered heat insulating time 3min; Treat that insulation finishes the back pressure relief; Be cooled to room temperature with the discharge plasma sintering stove, can obtain the block MgO pottery of ceramic crystalline grain average grain diameter less than 100nm.
Embodiment four
(1) pre-prepared of high-pressure sinter assembling die (sectional area approximately than be 4: 1)
(1) The Shanghai Toyo Tanso Co., Ltd. provides high-performance graphite material into the thermocouple inserted into the through hole has a size of:
The outer mold 1, size:
5 and the inner mold size:
external pressure head 2; would Nb-based superalloys (Nb-18Si-15W-10Mo) processing into a size:
metal laminations 4.
(2) adopt the plasma activated sintering method with ball mill mixing after the quality proportioning be 80: 15: 5 SiC, AlN and Lu
2O
3Powder sinters under the sintering condition of 300 ℃/min of heating rate, 1600 ℃ of sintering temperatures, sintering pressure 40MPa, sintered heat insulating time 5min and vacuum 12Pa respectively and is of a size of:
With
Disk, be used separately as ceramic lamination 3 and inner ram 6 after the processing through polishing again.
(2) the high pressure flash sintering method of nano ceramics
(1) the commercially available average grain diameter with 0.5g is the high-purity nm BaTiO of 30～50nm
3Ceramic powders is packed in the die cavity shown in Figure 17, and by the high-pressure sinter assembling die that assembles shown in Figure 1.
(2) with the above-mentioned nanometer BaTiO that is equipped with
3The high-pressure sinter assembling die of ceramic powders places the discharge plasma sintering stove to carry out sintering: 750 ℃ of 200 ℃/min of the rate of heat addition, sintering pressure 100MPa, sintering temperature; Sintered heat insulating time 3min; Treat that insulation finishes the back pressure relief; Be cooled to room temperature with the discharge plasma sintering stove, can obtain the block BaTiO of ceramic crystalline grain average grain diameter less than 100nm
3Pottery.
The present invention is not limited to above-mentioned specific embodiments; Above-mentioned specific embodiments only is schematic, guiding rather than restrictive; Each part dimension like the high-pressure sinter assembling die also can adopt other size that can be used for the plasma apparatus sintering; Supertherm also can adopt other Ni, Co and Nb base; Even supertherm such as Ti base, nano ceramics also comprises other single-phase or composite ceramicses, also comprises the silicon carbide ceramics that adopts the high strength and high conductivity that other sintering aids and sintering process prepare as the silicon carbide ceramics of ceramic lamination.
Claims (9)
1. high-pressure sinter assembling die; It is characterized in that: the assembled state of this mould does; The external mold (1) that comprises the hollow circular cylinder shape; The side of said external mold (1) is provided with the through hole (8) that thermocouple inserts; Be arranged on the internal mold (5) of the hollow circular cylinder shape in external mold (1) hollow cavity, the side of internal mold (5) is provided with the blind hole (9) that thermocouple inserts, and said external mold (1) and internal mold (5) are for tight fit and make the thermocouple of external mold (1) side insert the central lines of the thermocouple insertion blind hole (9) of through hole (8) and internal mold (5) side; Partly insert internal mold (5) the hollow cavity inner ram (6) of a pair of cylindrical shape at two ends up and down; The rounded face in said a pair of inner ram (6) the insertion internal mold (5) and the hollow cavity of internal mold (5) form die cavity (7), are arranged on the metallic laminations (4) of the outer a pair of cylindrical shape of a pair of inner ram (6), are arranged on the ceramic lamination (3) of the outer cylindrical shape of pair of metal lamination (4); Be arranged on the outer ram (2) of the outer cylindrical shape of a pair of ceramic lamination (3), said ceramic lamination (3) and outer ram (2) and external mold (1) tight fit.
2. assembling die according to claim 1 is characterized in that: the thermocouple that said external mold (1) side is provided with inserts through hole (8) and is positioned at middle position up and down, side.
3. assembling die according to claim 1 is characterized in that: the thermocouple that said internal mold (5) side is provided with inserts blind hole (9) and is positioned at middle position up and down, side.
4. according to claim 2 or 3 described assembling dies, it is characterized in that: said outer ram (2) is 4: 1～36: 1 with the ratio of the sectional area of inner ram (6).
5. according to claim 2 or 3 described assembling dies, it is characterized in that: said external mold (1), internal mold (5) and outer ram (2) material are graphite, and metallic laminations (4) material is a supertherm, and ceramic lamination (3) and inner ram (6) material are silicon carbide ceramics.
6. assembling die according to claim 5 is characterized in that: said supertherm be temperature resistant grade be more than 1000 ℃ Ni base, Co is basic, Nb is basic or the basic alloy of Ti.
7. assembling die according to claim 5 is characterized in that: said silicon carbide ceramics is for adopting AlN and Lu
2O
3For the pressure sintering of sintering aid form silicon carbide ceramics.
8. a high pressure flash sintering method for preparing nano ceramics is characterized in that: comprise the steps:
Step 1: nano ceramic powder is packed in the die cavity (7) of the said high-pressure sinter assembling die of claim 1, then the high-pressure sinter assembling die is assembled;
Step 2: the high-pressure sinter assembling die that nano ceramic powder will be housed places the plasma agglomeration stove to carry out sintering: rate of heat addition 100-300 ℃/min; Sintering pressure 100-1000MPa; Sintering temperature 500-800 ℃; Sintered heat insulating time 3-10min, insulation finishes the back pressure relief, is cooled to room temperature with the plasma agglomeration stove and gets final product.
9. method according to claim 8 is characterized in that: the average grain diameter of the described nano ceramic powder of step 1 is smaller or equal to 50nm.
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| CN102632238A (en) * | 2012-04-05 | 2012-08-15 | 华南师范大学 | Sintering mould |
| CN102721281A (en) * | 2012-05-17 | 2012-10-10 | 华南师范大学 | Simple sintering attachment for rapidly sintering block materials at an ultrahigh temperature |
| CN103819202A (en) * | 2014-01-14 | 2014-05-28 | 苏州永佳超硬耐磨材料有限公司 | Ceramic material sintering furnace and isostatic pressing field-controlled spark pulse sintering method |
| CN104525943A (en) * | 2014-11-21 | 2015-04-22 | 长安大学 | Pressurizing device for preparing high-density ultrafine grain tungsten block and application of pressurizing device |
| CN105904582A (en) * | 2016-06-08 | 2016-08-31 | 北京清能创新科技有限公司 | Multi-layer sintering mold and sintering method for boron carbide absorbers for nuclear reactor |
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