CN115194919A - Mold for preparing AlON transparent ceramic by SPS (semi-permeable plasma sintering), preparation method and obtained transparent ceramic - Google Patents

Mold for preparing AlON transparent ceramic by SPS (semi-permeable plasma sintering), preparation method and obtained transparent ceramic Download PDF

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Publication number
CN115194919A
CN115194919A CN202210920749.2A CN202210920749A CN115194919A CN 115194919 A CN115194919 A CN 115194919A CN 202210920749 A CN202210920749 A CN 202210920749A CN 115194919 A CN115194919 A CN 115194919A
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China
Prior art keywords
diameter
pressure head
die body
sleeve
cylinder
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CN202210920749.2A
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Chinese (zh)
Inventor
张朝晖
贾晓彤
程兴旺
徐天豪
冯向向
刘罗锦
刘娅
李先雨
王强
贾兆虎
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Tangshan Research Institute Of Beijing University Of Technology
Beijing Institute of Technology BIT
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Tangshan Research Institute Of Beijing University Of Technology
Beijing Institute of Technology BIT
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Priority to CN202210920749.2A priority Critical patent/CN115194919A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00—Moulds; Cores; Mandrels
    • B28B7/0097—Press moulds; Press-mould and press-ram assemblies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
    • B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • B28B17/02—Conditioning the material prior to shaping
    • B28B17/026—Conditioning ceramic materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00—Moulds; Cores; Mandrels
    • B28B7/0002—Auxiliary parts or elements of the mould
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00—Moulds; Cores; Mandrels
    • B28B7/40—Moulds; Cores; Mandrels characterised by means for modifying the properties of the moulding material
    • B28B7/46—Moulds; Cores; Mandrels characterised by means for modifying the properties of the moulding material for humidifying or dehumidifying
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina

Abstract

The invention discloses a mold for preparing AlON transparent ceramic by SPS, a preparation method and the obtained transparent ceramic. The die comprises a die body made of graphite materials and provided with a cavity, a hollow sleeve made of BN materials and capable of being sleeved in the cavity of the die body, an upper pressing head and a lower pressing head of the die body for encapsulating the die and the sleeve at two ends, and a gasket made of BN materials and positioned between the upper pressing head and the sleeve, the lower pressing head and the sleeve; the preparation method comprises the following steps: and adding the mixed powder or the green body of the raw materials into the die, and then performing vacuum sintering at 1500-1750 ℃ and post-treatment at 1550-1900 ℃ in an SPS sintering furnace to obtain the transparent ceramic. The AlON transparent ceramic can be prepared by one-step solid phase reaction sintering, the phenomenon of carbon pollution of the AlON transparent ceramic in the SPS sintering process is effectively avoided, and the optical transmittance of the AlON transparent ceramic is improved.

Description

Mold for preparing AlON transparent ceramic by SPS (semi-permeable plasma sintering), preparation method and obtained transparent ceramic
Technical Field
The invention relates to a preparation method of AlON transparent ceramic, in particular to a method for preparing AlON transparent ceramic according to SPS.
Background
Spinel type aluminum oxynitride (gamma-AlON) is Al 2 O 3 An important single-phase stable solid solution ceramic in an AlN system has the properties of high strength, high hardness, wear resistance, corrosion resistance, scratch resistance and the like, and has higher transmittance in visible light and infrared light bands, so that the ceramic is an ideal material for preparing transparent armors and infrared/visible windows.
At present, the AlON transparent ceramic is prepared by a two-step method, namely AlON powder is synthesized and then sintered at high temperature to densify the AlON transparent ceramic. The method for synthesizing AlON powder mainly comprises a solid-phase reaction method, an aluminothermic reduction nitridation method, a carbothermic reduction nitridation method and a self-propagating method; the high-temperature sintering method mainly comprises pressureless sintering, hot-pressing sintering, hot isostatic pressing sintering, microwave sintering and the like.
Compared with the traditional sintering method, the Spark Plasma Sintering (SPS) is used as a novel powder metallurgy sintering technology, has the advantages of high temperature rise speed, short sintering time, low sintering temperature, uniform heating, high production efficiency and the like, can densify ceramic powder at low temperature in short time, can inhibit the growth of crystal grains to a certain extent, keeps the microstructure of original particles, and improves the comprehensive mechanical property of a sintered body essentially. SPS technology can also enable Al 2 O 3 And AlN generates AlON transparent ceramic in one step through solid-phase reaction, so that the preparation process is greatly simplified, and the preparation time and the preparation cost are saved.
However, the existing method for preparing the AlON transparent ceramic by SPS sintering cannot eliminate carbon pollution on the product due to the limitation of the graphite mold used in the method. Carbon impurities in the AlON transparent ceramic can cause strong scattering of light to form scattering centers, the optical transmittance of the AlON transparent ceramic is seriously reduced, and the service performance of the product is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel mold capable of being applied to preparing AlON transparent ceramic by SPS and a method for preparing AlON transparent ceramic by adopting the mold through SPS, and the mold and the method can effectively avoid the phenomenon of carbon pollution generated when the conventional graphite mold is adopted to prepare AlON transparent ceramic by SPS in the prior art, so that AlON transparent ceramic which is free of carbon impurities and remarkably improved in transmittance is obtained.
The technical scheme of the invention is as follows:
a mold for preparing AlON transparent ceramics by SPS comprises a mold body which is provided with a cavity and is made of graphite materials, a hollow sleeve which is made of boron nitride ceramic materials (BN materials) and can be sleeved in the cavity of the mold body, an upper pressing head and a lower pressing head of the mold body which are used for packaging the mold and the sleeve at two ends, and a gasket made of boron nitride ceramic materials and arranged between the upper pressing head of the mold body, the lower pressing head of the mold body and the sleeve, wherein the inner diameter of the sleeve is equal to the diameter of the gasket.
Under the technical scheme, in the preparation process, the raw material powder or the blank can be added into the sleeve made of the BN material, and the raw material powder or the blank is effectively isolated from the die body pressure head made of the graphite material through the BN gasket, so that the carbon pollution of the graphite die to the product is fundamentally avoided; meanwhile, the mold has good heat conductivity, compressive strength and stress uniformity, so that the obtained product has compact structure, uniform texture and excellent mechanical property without being influenced by carbon pollution.
According to some preferred embodiments of the present invention, the mold body has a hollow cylindrical shape with a constant outer diameter, and the cavity thereof has a cylindrical shape; the sleeve is in a hollow cylindrical shape with equal outer diameter, and a hollow cavity of the sleeve is in a cylindrical shape; the outer diameter of the sleeve is equal to the inner diameter of the die body, namely the diameter of the cavity of the die body; the height of the sleeve is smaller than that of the die body; the structure, the shape and the size of the upper pressure head of the die body and the lower pressure head of the die body are the same, and the upper pressure head of the die body and the lower pressure head of the die body are both composed of two cylinders with different diameters, wherein the diameter of the cylinder with the large diameter of the upper pressure head of the die body or the lower pressure head of the die body is equal to the inner diameter of the die body, and the diameter of the cylinder with the small diameter of the upper pressure head of the die body or the lower pressure head of the die body is equal to the diameter of the gasket.
Considering that the SPS technique sinters the raw material powder or green body by pulse current heating, and the BN material used in the sleeve of the present invention is not conductive, in the above preferred embodiment, both ends of the sleeve of the BN material that can be embedded inside the graphite mold body are encapsulated by the same graphite encapsulating press head composed of two parts with different diameters. The large-diameter part of the pressure head can be in contact with the graphite die main body, so that the pulse current is ensured to be smoothly conducted, and sintering is completed; the small-diameter part of the pressure head can extend into the BN sleeve to finish pressure application, and the structure can not only ensure that the product is not polluted by carbon, but also ensure that SPS sintering is effectively carried out.
According to some of its more preferred embodiments, the sleeve has an inner diameter of 20mm, a wall thickness of 3mm and a height of 40mm; the diameter of the cylindrical cavity of the die body is 26.05mm, the wall thickness is 15mm, and the height is 80mm; the diameter of the large-diameter cylinder of the upper pressure head of the die body or the lower pressure head of the die body is 26mm, the height of the large-diameter cylinder is 25mm, and the diameter of the small-diameter cylinder is 19.95mm, and the height of the small-diameter cylinder is 20mm; the diameter of the gasket is 19.95mm, and the thickness is 3mm.
According to some preferred embodiments of the present invention, the mold body has a hollow cylindrical shape with two ends having the same outer diameter; the cavity is of a three-section structure and comprises an upper cylindrical structure with a larger diameter, a lower cylindrical structure with a smaller diameter and a truncated cone-shaped structure which connects the upper cylindrical structure and the lower cylindrical structure and has a larger diameter at one end and a smaller diameter at the other end, wherein the upper cylindrical structure and the lower cylindrical structure are equal in height; the shape and the height of the sleeve are the same as those of the circular truncated cone-shaped structure; the hollow cavity of the sleeve is cylindrical; the die body upper pressure head and the die body lower pressure head are both composed of two cylinders with different diameters, wherein the diameter of the cylinder with the large diameter of the die body upper pressure head is equal to the large diameter of the truncated cone-shaped structure, the diameter of the cylinder with the small diameter of the die body upper pressure head is equal to the diameter of the gasket, the diameter of the cylinder with the large diameter of the die body lower pressure head is equal to the small diameter of the truncated cone-shaped structure, and the diameter of the cylinder with the small diameter of the die body lower pressure head is equal to the diameter of the gasket; the height of the large-diameter cylinder of the upper press head of the die body is equal to that of the large-diameter cylinder of the lower press head of the die body, and the height of the small-diameter cylinder of the upper press head of the die body is equal to that of the small-diameter cylinder of the lower press head of the die body.
Under the preferred embodiment, the truncated cone-shaped structure of the cavity of the die body can better support the sleeve of the truncated cone-shaped structure and can bear higher sintering pressure, so that a higher sintering driving force can be provided in the preparation process, and further promotion effect on sintering of the AlON transparent ceramic is achieved.
According to some preferred embodiments thereof, the sleeve has an inner diameter of 17mm, outer diameters at both ends of 27mm and 37mm, respectively, and a height of 40mm; the diameters of the two ends of the truncated cone-shaped structure are 27.05mm and 37.05mm respectively; the diameters of the upper cylindrical structure and the lower cylindrical structure are 37.05 and 27.05mm respectively; the total height of the die body is 80mm; the diameter of the large-diameter cylinder of the pressure head on the die body is 37mm, the height of the large-diameter cylinder is 25mm, and the diameter of the small-diameter cylinder is 16.95mm, and the height of the small-diameter cylinder is 20mm; the diameter of the large-diameter cylinder of the lower pressure head of the die body is 27mm, the height of the large-diameter cylinder is 25mm, and the diameter of the small-diameter cylinder is 16.95mm, and the height of the small-diameter cylinder is 20mm; the gasket has a diameter of 16.95mm and a thickness of 2mm.
According to some preferred embodiments of the invention, the inner diameter of the sleeve is 5 to 60mm, and/or the wall thickness of the sleeve is 1 to 40mm, and/or the height of the sleeve is 20 to 80mm, and/or the thickness of the spacer is 1 to 10mm.
The present invention further provides a method for preparing AlON transparent ceramic by SPS using the above mold, which comprises:
(1) The molar ratio is (55-70): (45 to 30) Al 2 O 3 Mixing and ball-milling the powder, alN powder and sintering aid to obtain mixed powder;
(2) Directly adding the mixed powder or the screened powder after screening the mixed powder into the mold, or firstly pressing the mixed powder into a blank and then adding the blank into the mold to obtain a combination body to be sintered;
(3) Putting the assembly to be sintered into an SPS sintering furnace for vacuum sintering, wherein the sintering temperature rise rate is 50-300 ℃/min, the sintering temperature is 1500-1750 ℃, the sintering pressure is 5-60 MPa, the heat preservation time is 1-30 min, and then cooling along with the furnace to obtain a sintered body;
(4) And taking out the sintered body, and then carrying out heat treatment in an inert atmosphere to obtain the AlON transparent ceramic, wherein the heat treatment temperature is 1550-1900 ℃, and the heat preservation time is 0.5-6 h.
According to some preferred embodiments of the invention, the method further comprises: and (4) grinding and/or polishing the AlON transparent ceramic obtained in the step (4).
According to some preferred embodiments of the invention, the sintering aid comprises Y 2 O 3 、MgO、La 2 O 3 One or more of (a).
According to some preferred embodiments of the present invention, the mixing ball milling is performed by an all-directional planetary ball mill.
According to some preferred embodiments of the present invention, the step (2) is performed after the mixed powder is dried.
According to some preferred embodiments of the invention, the screen is 200 mesh standard screen.
The invention further provides the AlON transparent ceramic prepared by the method.
The obtained transparent ceramic effectively avoids carbon pollution to the transparent ceramic caused by the graphite mold, and the transmittance of the transparent ceramic can reach more than 70%.
The invention has the following beneficial effects:
(1) The preparation method of the invention can obtain AlON ceramic raw material powder with good dispersion and uniform components without adding any dispersant in the ball milling process, thereby effectively avoiding secondary pollution of the dispersant to the product.
(2) The preparation method of the invention utilizes the novel SPS technology to obtain the AlON transparent ceramic through one-step solid-phase reaction sintering, reduces the sintering temperature, shortens the heat preservation time and improves the production efficiency while simplifying the preparation process.
(3) The preparation mold effectively avoids carbon pollution of the graphite mold to the AlON transparent ceramic in the SPS sintering process, and improves the optical transmittance of the obtained AlON transparent ceramic.
Drawings
FIG. 1 is a cross-sectional assembly view of a graphite mold used in the prior art;
fig. 2 is a sectional assembly view of a first tooling die of the present invention according to an embodiment.
Fig. 3 is a sectional assembly view of a second type of working mold according to the present invention in an embodiment.
Fig. 4 is a structural view of a mold body of a conventional mold used in a comparative example.
Fig. 5 is a structural view of an indenter of a conventional die used in a comparative example.
Fig. 6 is a structural view of a mold body of the first working mold used in example 1.
Fig. 7 is a structural view of a die body ram of the first working die used in example 1.
Fig. 8 is a structural view of a sleeve of the first working mold used in example 1.
Fig. 9 is a structural view of a shim of the first working mold used in example 1.
Fig. 10 is a structural view of a mold body of a second working mold used in example 2.
Fig. 11 is a structural view of the ram on the die body of the second working die used in example 2.
Fig. 12 is a structural view of a lower ram of the die body of the second working die used in example 2.
Fig. 13 is a structural view of a sleeve of the second working mold used in example 2.
Fig. 14 is a structural view of a shim of the second working mold used in example 2.
FIG. 15 is a graph showing transmittance curves of AlON ceramic samples in comparative examples;
FIG. 16 is a graph of transmittance of AlON ceramic samples of example 1;
fig. 17 is a transmittance curve of an AlON ceramic sample of example 2.
Detailed Description
The present invention is described in detail with reference to the following embodiments and drawings, but it should be understood that the embodiments and drawings are only for illustrative purposes and are not intended to limit the scope of the present invention. All reasonable variations and combinations included within the spirit of the invention are within the scope of the invention.
Referring to fig. 1, a graphite mold of the prior art includes a hollow cylinder made of graphite having a cylindrical cavity, i.e., a mold body 101, and two cylindrical press heads 102 which are inserted into the mold body to enclose both ends thereof. When AlON ceramic is prepared, al is required to be filled into the die 2 O 3 And AlN raw material powderAnd sintering aid, which is then placed into an SPS sintering furnace for vacuum sintering after being packaged by a pressure head. In the process, the raw material powder 103 is in direct contact with the graphite mold, which causes carbon pollution to the product.
In contrast, the processing mold of the present invention shown in fig. 2 and 3 includes a mold body made of graphite and having a hollow cavity, an upper pressing head and a lower pressing head made of graphite which can be inserted into the mold body to encapsulate both ends of the mold body, a hollow sleeve made of BN material which can be inserted into the cavity of the mold body, and a gasket made of BN material for preventing the graphite pressing head from directly contacting with the raw material powder, and specifically includes:
a first processing mold as shown in fig. 2, wherein the mold body 201 is a hollow cylinder with a constant outer diameter, and the cavity in the cylindrical mold body 201 is also a cylinder; the sleeve 202 is a hollow cylinder with equal outer diameter, the outer diameter of the sleeve is equal to the inner diameter of the die body 201, namely the diameter of the cavity of the die body 201, the cavity of the cylindrical sleeve 202 is also cylindrical, and the height of the sleeve 202 is smaller than that of the die body 201; the upper pressure head 203 of the die body and the lower pressure head 204 of the die body have the same structure, shape and size and are composed of two cylinders with different diameters, wherein the diameter of the cylinder with the large diameter of the upper pressure head 203 or the lower pressure head 204 of the die body is equal to the inner diameter of the die body 201, namely the outer diameter of the sleeve 202, the diameter of the cylinder with the small diameter of the upper pressure head 203 or the lower pressure head 204 of the die body is equal to the inner diameter of the gasket 205, namely the sleeve 202, and the raw material powder or blank 206 is positioned in the sleeve 202 and is separated from the upper pressure head 203 of the die body and the lower pressure head 204 of the die body by the upper gasket 205 and the lower gasket 205.
A second processing mold as shown in fig. 3, wherein the mold body 301 is a hollow cylinder with two ends having the same outer diameter, and the cavity in the cylindrical mold body 301 is a three-section structure including an upper cylindrical structure with a larger diameter, a lower cylindrical structure with a smaller diameter, and a truncated cone structure connecting the upper cylindrical structure and the lower cylindrical structure, wherein the upper cylindrical structure and the lower cylindrical structure have the same height; the shape and the height of the sleeve 302 are the same as those of the round table-shaped structure, and the hollow cavity of the sleeve 302 is cylindrical; the upper die body ram 303 and the lower die body ram 304 are both composed of two cylinders with different diameters, wherein the diameter of the cylinder with the large diameter of the upper die body ram 303 is equal to the diameter of the larger end of the circular truncated cone-shaped structure, namely the larger outer diameter of the sleeve 302, the diameter of the cylinder with the small diameter of the upper die body ram 303 is equal to the inner diameter of the gasket 305, namely the sleeve 302, the diameter of the cylinder with the large diameter of the lower die body ram 304 is equal to the diameter of the smaller end of the circular truncated cone-shaped structure, namely the smaller outer diameter of the sleeve 302, and the diameter of the cylinder with the small diameter of the lower die body ram 304 is equal to the diameter of the gasket 305, namely the inner diameter of the sleeve 302; the height of the large-diameter cylinder of the upper ram 303 of the die body is equal to that of the large-diameter cylinder of the lower ram 304 of the die body, the height of the small-diameter cylinder of the upper ram 303 of the die body is equal to that of the small-diameter cylinder of the lower ram 304 of the die body, and the raw material powder or blank 306 is positioned in the sleeve 302 and separated from the upper ram 303 of the die body and the lower ram 304 of the die body by two upper and lower spacers 305.
It should be understood that the equality in the above embodiments is based on engineering practice, i.e. it does not require strict mathematical equality, but may have a certain deviation under consideration of the actual assembly effect of the mold, as in the second type of processing mold, when the outer diameters of the two ends of the sleeve are 27mm and 37mm respectively, the diameters of the two ends of the truncated cone-shaped structure accommodating the sleeve are 27.05mm and 37.05mm respectively.
The use of the processing die is as follows: the sleeve is placed into the die body, then the lower pressing head of the die body is inserted, one end of the sleeve and one end of the die body are closed, the BN gasket used for isolating the pressing head of the die body from raw material powder is placed, the raw material powder to be sintered is added into the sleeve from the other end, the BN gasket is continuously placed above the powder, then the upper pressing head of the die body is used for closing the other ends of the sleeve and the die body, packaging is completed, and the assembly to be sintered is formed.
In the above embodiment, the sleeve has an inner diameter of preferably 5 to 60mm, a wall thickness of preferably 1 to 40mm, a height of preferably 20 to 80mm, and a gasket thickness of preferably 1 to 10mm.
According to the above processing mold, some embodiments of the method for preparing AlON transparent ceramic by SPS of the present invention include the steps of:
(1) The molar ratio is (55-70): (45 to 30) Al 2 O 3 Mixing and ball-milling the powder, alN powder and sintering aid to obtain mixed powder;
(2) Directly adding the mixed powder or the screened mixed powder into the processing mould, or firstly pressing the mixed powder into a blank and then adding the blank into the processing mould;
(3) Putting the assembled mould into an SPS sintering furnace for vacuum sintering, wherein the sintering temperature rise rate is 50-300 ℃/min, the sintering temperature is 1500-1750 ℃, the sintering pressure is 5-60 MPa, and the temperature is kept for 1-30 min and then the mould is cooled along with the furnace to obtain a sintered body;
(4) And taking out the obtained sintered body, and then carrying out heat treatment in an inert atmosphere to obtain the AlON transparent ceramic, wherein the heat treatment temperature is 1550-1900 ℃, and the treatment time is preferably 0.5-6 h.
In some preferred embodiments, the above preparation method may further comprise:
(5) And (5) grinding and/or polishing the AlON transparent ceramic sample obtained in the step (4).
It may also include one or more of the following preferred embodiments:
the sintering aid comprises Y 2 O 3 、MgO、La 2 O 3 One or more of (a).
The mixing ball milling is realized by an all-directional planetary ball mill, and/or a nylon ball milling tank is used.
The mixed powder is dried and then subjected to the step (2), and the drying can be realized by using a rotary evaporator, for example.
And screening the mixed powder to obtain the screened mixed powder, and screening the mixed powder through a standard sieve of 200 meshes.
The technical solution of the present invention is further shown in the following embodiments.
Comparative example
Preparing AlON transparent ceramic by the following steps:
(1) Powder mixing: in a molar ratio of 60mol%:40mol% of Al 2 O 3 The powder and AlN powder as raw materials, and a sintering aid (Y) 2 O 3 、MgO、La 2 O 3 One or more of the above) are added into a nylon ball milling tank together, and an omnibearing planetary ball mill is adopted to perform ball milling and mixing on the powder;
(2) Drying and sieving: drying the mixed powder obtained in the step (1) by using a rotary evaporator, and sieving the dried powder through a 200-mesh standard sieve to obtain uniformly dispersed mixed powder;
(3) Die filling: filling the uniformly dispersed mixed powder obtained in the step (2) into a graphite mould filled with 1-2 layers of graphite paper;
(4) Spark plasma sintering: placing the mould filled with the mixed powder into an SPS sintering furnace for vacuum sintering, wherein the heating rate is 100 ℃/min, the sintering temperature is 1600 ℃, the sintering pressure is 30MPa, and carrying out furnace cooling after heat preservation for 5min to obtain an AlON ceramic sample;
(5) And (3) post-treatment: placing the AlON ceramic sample obtained in the step (4) in N 2 Processing under the condition that the processing temperature is 1800 ℃ and the processing time is 2h;
(6) Grinding and polishing: and (5) grinding and polishing the AlON ceramic sample obtained in the step (5) to obtain the AlON transparent ceramic.
The structure of the used die is shown in fig. 4-5, and the size is as follows:
the inner diameter of the die body is 20.2mm, the wall thickness is 15mm, the height is 60mm, and the diameter of the cylindrical pressure head is 20mm and the height is 30mm.
The transmittance test of the AlON transparent ceramic obtained was performed, and the transmittance curve obtained by the transmittance test was as shown in fig. 15, and the transmittance at a wavelength of 1500nm was 52.48%.
Example 1
AlON transparent ceramics were carried out by the same steps (1) to (2) and (6) as in the comparative examples, and the steps (3) to (5) were as follows:
(3) Die filling: putting the uniformly dispersed mixed powder obtained in the step (2) into a mould;
(4) Spark plasma sintering: placing the mould filled with the mixed powder into an SPS sintering furnace for vacuum sintering, wherein the heating rate is 150 ℃/min, the sintering temperature is 1650 ℃, the sintering pressure is 20MPa, and carrying out heat preservation for 5min and then cooling along with the furnace to obtain an AlON ceramic sample;
(5) And (3) post-treatment: placing the AlON ceramic sample obtained in the step (4) in N 2 The treatment is carried out under the conditions that the treatment temperature is 1700 ℃ and the treatment time is 3h.
The structure of the die is shown in fig. 6-9, and the dimensions are as follows:
the BN sleeve is cylindrical, the inner diameter is 20mm, the wall thickness is 3mm, and the height is 40mm.
The diameter of the cylindrical cavity of the graphite mold body is 26.05mm, the wall thickness is 15mm, and the total height is 80mm.
The pressure head is of a shape with wide upper part and narrow lower part, and the sizes of the upper pressure head and the lower pressure head are the same. The major diameter of the pressure head is 26mm, the height of the major diameter part is 25mm, the minor diameter of the pressure head is 19.95mm, and the height of the minor diameter part is 20mm.
The diameter of the BN gasket is 19.95mm, and the thickness of the BN gasket is 3mm.
The transmittance test of the AlON transparent ceramic obtained by the method is carried out, the transmittance curve is shown in figure 16, the transmittance of the AlON transparent ceramic at the wavelength of 1500nm is 74.41 percent, and the transmittance is improved by 41.79 percent compared with the transmittance of the AlON transparent ceramic in the comparative example.
Example 2
AlON transparent ceramics were carried out by the same procedures (1) to (2) and procedures (4) to (6) as in the comparative examples, and the procedure (3) was as follows:
(3) Die filling: and (3) performing dry pressing forming on the uniformly dispersed mixed powder obtained in the step (2) at the first time of 20MPa, performing cold isostatic pressing forming at the second time of 250MPa to obtain a pressed blank, and then filling the pressed blank into a die.
The structure of the used mould is shown in figures 10-14, and the dimensions are as follows:
the BN sleeve is in a circular truncated cone shape, the inner diameter of the BN sleeve is 17mm, the outer diameters of two ends of the BN sleeve are respectively 27mm and 37mm, and the height of the BN sleeve is 40mm.
The diameters of two ends of the truncated cone-shaped cavity in the middle part of the graphite mould body are respectively 27.05mm and 37.05mm.
The diameters of the cylindrical cavities at the upper part and the lower part in the graphite mould body are respectively the same as the diameters of two ends of the truncated cone-shaped cavity, namely 37.05 and 27.05mm, and the total height of the mould body is 80mm.
The pressure head is of a type with wide upper part and narrow lower part, and the sizes of the upper pressure head and the lower pressure head are different. The large diameter of the upper pressure head is 37mm, the height of the large diameter part is 25mm, the small diameter of the upper pressure head is 16.95mm, and the height of the small diameter part is 20mm; the major diameter of the lower pressure head is 27mm, the height of the major diameter part is 25mm, the minor diameter of the lower pressure head is 16.95mm, and the height of the minor diameter part is 20mm.
The diameter of the BN gasket is 16.95mm, and the thickness of the BN gasket is 2mm.
The transmittance test of the obtained AlON transparent ceramic was carried out, and the transmittance curve obtained is shown in fig. 17, and the transmittance at the wavelength of 1500nm is 76.13%, which is improved by 45.06% compared with the transmittance of the AlON transparent ceramic in the comparative example.
The present invention includes, but is not limited to, the above embodiments, and any modifications, additions, equivalents, or local improvements made under the principle of the present invention are considered to be within the scope of the present invention.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.

Claims (10)

1. The mold for preparing the AlON transparent ceramic through the SPS is characterized by comprising a mold body, a hollow sleeve, an upper mold body pressure head, a lower mold body pressure head and a gasket, wherein the mold body is provided with a cavity and made of graphite materials, the hollow sleeve can be sleeved in the cavity of the mold body and made of boron nitride ceramic materials, the upper mold body pressure head and the lower mold body pressure head are used for sealing the mold and the sleeve at two ends, the gasket is located between the upper mold body pressure head, the lower mold body pressure head and the sleeve and made of the boron nitride ceramic materials, and the inner diameter of the sleeve is equal to the diameter of the gasket.
2. The mold according to claim 1, wherein the mold body is a hollow cylinder of constant outer diameter, the cavity of which is cylindrical; the sleeve is in a hollow cylindrical shape with equal outer diameter, and a hollow cavity of the sleeve is in a cylindrical shape; the outer diameter of the sleeve is equal to the inner diameter of the die body, namely the diameter of the cavity of the die body; the height of the sleeve is smaller than that of the die body; the structure, the shape and the size of the upper pressure head of the die body and the lower pressure head of the die body are the same, and the upper pressure head of the die body and the lower pressure head of the die body are both composed of two cylinders with different diameters, wherein the diameter of the cylinder with the large diameter of the upper pressure head of the die body or the lower pressure head of the die body is equal to the inner diameter of the die body, and the diameter of the cylinder with the small diameter of the upper pressure head of the die body or the lower pressure head of the die body is equal to the diameter of the gasket.
3. The mold according to claim 1, wherein the mold body is a hollow cylinder with equal outer diameters at both ends; the cavity is of a three-section structure and comprises an upper cylindrical structure with a larger diameter, a lower cylindrical structure with a smaller diameter and a truncated cone-shaped structure which connects the upper cylindrical structure and the lower cylindrical structure and has a larger diameter at one end and a smaller diameter at the other end, wherein the upper cylindrical structure and the lower cylindrical structure are equal in height; the shape and the height of the sleeve are the same as those of the circular truncated cone-shaped structure; the hollow cavity of the sleeve is cylindrical; the die body upper pressure head and the die body lower pressure head are respectively composed of two cylinders with different diameters, wherein the diameter of the cylinder with the large diameter of the die body upper pressure head is equal to the large diameter of the circular truncated cone-shaped structure, the diameter of the cylinder with the small diameter of the die body upper pressure head is equal to the diameter of the gasket, the diameter of the cylinder with the large diameter of the die body lower pressure head is equal to the small diameter of the circular truncated cone-shaped structure, and the diameter of the cylinder with the small diameter of the die body lower pressure head is equal to the diameter of the gasket; the height of the large-diameter cylinder of the upper pressure head of the die body is equal to that of the large-diameter cylinder of the lower pressure head of the die body, and the height of the small-diameter cylinder of the upper pressure head of the die body is equal to that of the small-diameter cylinder of the lower pressure head of the die body.
4. A mould according to any one of claims 1 to 3, wherein the sleeve has an internal diameter of from 5 to 60mm, and/or the sleeve has a wall thickness of from 1 to 40mm, and/or the sleeve has a height of from 20 to 80mm, and/or the shim has a thickness of from 1 to 10mm.
5. The die of claim 2, wherein the sleeve has an inner diameter of 20mm, a wall thickness of 3mm, and a height of 40mm; the diameter of the cylindrical cavity of the die body is 26.05mm, the wall thickness is 15mm, and the height is 80mm; the diameter of the large-diameter cylinder of the upper pressure head of the die body or the lower pressure head of the die body is 26mm, the height of the large-diameter cylinder is 25mm, and the diameter of the small-diameter cylinder is 19.95mm, and the height of the small-diameter cylinder is 20mm; the diameter of the gasket is 19.95mm, and the thickness is 3mm.
6. A mould according to claim 3, wherein the sleeve has an internal diameter of 17mm, an external diameter at each end of 27mm and 37mm respectively, and a height of 40mm; the diameters of the two ends of the truncated cone-shaped structure are 27.05mm and 37.05mm respectively; the diameters of the upper cylindrical structure and the lower cylindrical structure are 37.05 and 27.05mm respectively; the total height of the die body is 80mm; the diameter of the large-diameter cylinder of the pressure head on the die body is 37mm, the height of the large-diameter cylinder is 25mm, and the diameter of the small-diameter cylinder is 16.95mm, and the height of the small-diameter cylinder is 20mm; the diameter of the large-diameter cylinder of the lower pressure head of the die body is 27mm, the height of the large-diameter cylinder is 25mm, and the diameter of the small-diameter cylinder is 16.95mm, and the height of the small-diameter cylinder is 20mm; the gasket has a diameter of 16.95mm and a thickness of 2mm.
7. A method for preparing AlON transparent ceramic by SPS using the mold of any one of claims 1 to 6, comprising:
(1) The molar ratio is (55-70): (45 to 30) Al 2 O 3 Mixing and ball-milling the powder, alN powder and sintering aid to obtain mixed powder;
(2) Directly adding the mixed powder or the screened powder after screening the mixed powder into the mold, or firstly pressing the mixed powder into a blank and then adding the blank into the mold to obtain a combination body to be sintered;
(3) Putting the assembly to be sintered into an SPS sintering furnace for vacuum sintering, wherein the sintering temperature rise rate is 50-300 ℃/min, the sintering temperature is 1500-1750 ℃, the sintering pressure is 5-60 MPa, the heat preservation time is 1-30 min, and then cooling along with the furnace to obtain a sintered body;
(4) And carrying out heat treatment on the sintered body in an inert atmosphere to obtain the AlON transparent ceramic, wherein the heat treatment temperature is 1550-1900 ℃, and the heat preservation time is 0.5-6 h.
8. The method of claim 7, further comprising: and (4) grinding and/or polishing the AlON transparent ceramic obtained in the step (4).
9. The method of claim 7, wherein the sintering aid comprises Y 2 O 3 、MgO、La 2 O 3 One or more of; and/or the mixing ball milling is realized by an all-directional planetary ball mill; and/or, drying the mixed powder and then performing the step (2); and/or, the screen is 200-mesh standard screen.
10. An AlON transparent ceramic prepared according to the method of any one of claims 7 to 9.
CN202210920749.2A 2022-08-02 2022-08-02 Mold for preparing AlON transparent ceramic by SPS (semi-permeable plasma sintering), preparation method and obtained transparent ceramic Pending CN115194919A (en)

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Publication number Priority date Publication date Assignee Title
CN203184649U (en) * 2013-04-26 2013-09-11 河南科技大学 Hot pressing sintering mold
CN103896601A (en) * 2014-03-06 2014-07-02 清华大学 Hot pressed sintering method of ceramic products with high density and complex shapes
CN205200540U (en) * 2015-12-08 2016-05-04 河南科技大学 Spark plasma sintering mould and use sintering equipment of this mould
JP2018008833A (en) * 2016-07-11 2018-01-18 住友金属鉱山株式会社 Spacer for discharge plasma sintering, discharge plasma sintering device, and discharge plasma sintering method
FR3076242A1 (en) * 2017-12-28 2019-07-05 Safran Ceramics PROCESS FOR MANUFACTURING A PIECE OF COMPOSITE MATERIAL BY INJECTING POWDER IN A FIBROUS REINFORCEMENT WITH COMPOSITE FILTRATION STRATE DRAINAGE
CN112358296A (en) * 2014-08-14 2021-02-12 清华大学 Preparation method of gadolinium oxysulfide scintillating ceramic
CN216325088U (en) * 2021-08-10 2022-04-19 美尔森先进石墨（昆山）有限公司 Graphite mould for spark plasma sintering
CN114538931A (en) * 2022-03-11 2022-05-27 北京理工大学 High-performance AlON transparent ceramic and low-temperature rapid preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203184649U (en) * 2013-04-26 2013-09-11 河南科技大学 Hot pressing sintering mold
CN103896601A (en) * 2014-03-06 2014-07-02 清华大学 Hot pressed sintering method of ceramic products with high density and complex shapes
CN112358296A (en) * 2014-08-14 2021-02-12 清华大学 Preparation method of gadolinium oxysulfide scintillating ceramic
CN205200540U (en) * 2015-12-08 2016-05-04 河南科技大学 Spark plasma sintering mould and use sintering equipment of this mould
JP2018008833A (en) * 2016-07-11 2018-01-18 住友金属鉱山株式会社 Spacer for discharge plasma sintering, discharge plasma sintering device, and discharge plasma sintering method
FR3076242A1 (en) * 2017-12-28 2019-07-05 Safran Ceramics PROCESS FOR MANUFACTURING A PIECE OF COMPOSITE MATERIAL BY INJECTING POWDER IN A FIBROUS REINFORCEMENT WITH COMPOSITE FILTRATION STRATE DRAINAGE
CN216325088U (en) * 2021-08-10 2022-04-19 美尔森先进石墨（昆山）有限公司 Graphite mould for spark plasma sintering
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