CN105936595A - Silicon nitride heating element and preparation method thereof - Google Patents

Silicon nitride heating element and preparation method thereof Download PDF

Info

Publication number
CN105936595A
CN105936595A CN201510841326.1A CN201510841326A CN105936595A CN 105936595 A CN105936595 A CN 105936595A CN 201510841326 A CN201510841326 A CN 201510841326A CN 105936595 A CN105936595 A CN 105936595A
Authority
CN
China
Prior art keywords
silicon nitride
powder
weight
sintering
blank
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510841326.1A
Other languages
Chinese (zh)
Inventor
曾小锋
李勇全
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hengyang Kai Xin Special Material Science And Technology Ltd
Original Assignee
Hengyang Kai Xin Special Material Science And Technology Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hengyang Kai Xin Special Material Science And Technology Ltd filed Critical Hengyang Kai Xin Special Material Science And Technology Ltd
Priority to CN201510841326.1A priority Critical patent/CN105936595A/en
Publication of CN105936595A publication Critical patent/CN105936595A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/584—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 silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
    • C04B35/6264—Mixing media, e.g. organic solvents
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
    • C04B41/5062—Borides, Nitrides or Silicides
    • C04B41/5066—Silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3821—Boron carbides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3865—Aluminium nitrides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/656—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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/658—Atmosphere during thermal treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/661—Multi-step sintering
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/788—Aspect ratio of the grains
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention discloses a silicon nitride heating element and a preparation method thereof. The silicon nitride heating element is composed of a heating source and a heating body; the heating source is tungsten wire, and the heating body is prepared from raw materials of, by weight, 80-95 parts of silicon nitride (Si3N4), 0.1-5 parts of aluminum oxide (Al2O3), 2-8 parts of yttrium oxide (Y2O3) and 3-5 parts of aluminum nitride (A1N) by grinding, mold pressing and high temperature sintering. The silicon nitride heating element produced by the method has the advantages of high reliability and safety, increased fracture toughness and increased bending strength.

Description

A kind of silicon nitride heat generating body and preparation method thereof
Technical field
The present invention relates to heating technical field, relate in particular to a kind of silicon nitride heat generating body and preparation method thereof.
Background technology
Silicon nitride is a kind of covalent bond pottery, pure Si3N4Powder body cannot sinter, it is necessary to adds a small amount of sintering aid in high temperature shape Become liquid phase, carry out liquid-phase sintering, just can obtain the silicon nitride material of excellent performance.Conventional additive includes: A1203、MgO、 Si02Deng metal-oxide, Y203、La203、 Ce02Deng rare earth oxide, and A1N, Mg3N2, the nitride such as TiN, ZrN.Gao Xing Can silicon nitride ceramics have the electricity of excellence such as insulation, high-strength, high temperature resistant, resistance to oxidation, heat shock resistance and high-termal conductivity, calorifics and Mechanical property.
Silicon nitride heating plate is that one combines high-performance silicon nitride ceramics matrix and long-life powerful high-temperature metal is sent out The device of heated filament.Having volume little, power is big and thermal efficiency high, while be also proved to be a kind of safe and reliable heating Mode.After direct-electrifying, temperature is done on surface can reach 1200 degrees Celsius, and working life is up to more than 5000 hours.High temperature Metal heating wire material includes, the material such as tungsten filament, molybdenum filament and various tungsten-molybdenum alloy silks.
At present, more there is the phenomenon of carburizing in the silicon nitride heating sheet material in market, surface distributed has bulk black from the appearance The phenomenon such as speckle, black patch, color and luster is uneven.Pure Si3N4The true qualities of dense sintering material should be canescence, and existing product exists mostly Matrix color turns black, and surface is uniformly or non-uniformly distributed pore, more has surface distributed to have the phenomenons such as bulk black speck, black patch.This Mainly directly contacting with graphite due to blank during hot pressed sintering, carbon penetrates into along liquid channel, dissolves in liquid phase, Or with silicon nitride react produce.The infiltration of carbon can deteriorate the insulating properties of material, reduces safety and reliability. Simultaneously because the hot pressed sintering time is short, relying on the mechanical pressure fine and close effect of strengthening, the material obtained exists that boundary stress is big, liquid phase The microstructure that crystallization is insufficient, affects the service life of matrix material.
Summary of the invention
Present invention aims to the defect of above-mentioned prior art, it is provided that a kind of silicon nitride heat generating body and preparation side thereof Method, the silicon nitride heat generating body using the method to be produced has higher reliability and safety.
To achieve these goals, the technical scheme is that
A kind of silicon nitride heat generating body, it is made up of pyrotoxin and heating body, and described pyrotoxin is tungsten filament, described heating body with Silicon nitride (Si3N4), aluminium sesquioxide (A1203), yttrium oxide (Y203), aluminium nitride (A1N) be raw material, be formulated grinding, Compression molding, high temperature sintering form, and in terms of the gross weight of raw material, in raw material, the parts by weight of name component are:
Silicon nitride (Si3N4) 80～95
Aluminium sesquioxide (A1203) 0.1～5
Yttrium oxide (Y203) 2～8
Aluminium nitride (A1N) 3～5
Boron carbide (B4C) 1～3.
As the improvement to technique scheme, in raw material, the parts by weight of name component are:
Silicon nitride (Si3N4) 90
Aluminium sesquioxide (A1203) 3
Yttrium oxide (Y203) 5
Aluminium nitride (A1N) 4
Boron carbide (B4C) 2.
Invention additionally provides a kind of raw material by above-mentioned formula and make the preparation method of silicon nitride heat generating body, this is prepared The step of method is:
S1, by silicon nitride powder, aluminium sesquioxide powder, yttrium oxide powder, aluminium nitride powder, boron carbide powder by each Parts by weight carry out proportioning mixing, by compound and high-temperature liquid-phase sintering aid by weight 0.80～0.90:0.02～0.04 Ratio insert in dehydrated alcohol and mix, batch mixing ground after 24～72 hours, made formulation material through mist projection granulating；
S1, by after dry-pressing formed for described formulation material, the isostatic cool pressing by 200～250MPa is the most compressing, and pressurize 5 ～10 minutes, to make blank；
S3, uniformly coat one layer of boron nitride sealing coat post-drying at described blank surface；
S4, then carry out hot pressed sintering, sintering pressure 20～50MPa, sintering temperature 1700～1950 DEG C, temperature retention time 1～5 Hour, to make blank；
S5, described blank is put in vacuum atmosphere oven, keep 1200～1500 DEG C of constant temperature 10～24 hours, then natural cooling To room temperature.
As the improvement to technique scheme, described boron nitride sealing coat is to be mixed by boron nitride powder and silicon nitride powder The thick shape slurry reconciled into dehydrated alcohol after conjunction；Wherein, silicon nitride powder with the part by weight of boron nitride powder is: 0.10: 0.90～1.00.
As the improvement to technique scheme, in described step 4, when carrying out hot pressed sintering, the hot pressed sintering of employing Mould is hot pressing graphite jig.
As the improvement to technique scheme, when being hot pressed sintering mould using hot pressing graphite jig, hot pressing graphite Mould scribbles one layer of described boron nitride sealing coat on the contact surface of blank.
Compared with prior art, the present invention has the advantage that with good effect and is:
The silicon nitride heat generating body of the present invention, uses high purity silicon nitride (Si3N4) powder body, a small amount of high-temperature liquid-phase sintering aid and three oxidation Two aluminium powder material, yttrium oxide powder, aluminium nitride powder, boron carbide powder form, through blank molding, hot pressed sintering and high temperature Compact silicon nitride base heater is made after heat treatment.This heater has high-strength, highly thermally conductive, the feature of high reliability.Wherein hair Base surface has boron nitride powder (BN) coating, this process eliminates the infiltration of carbon in production process.High-temperature heat treatment work Skill eliminates material stress, promotes the crystallization of grain boundary glassy phase, substantially increases reliability and the safety of device.Hot pressing is burnt Knot, aluminium sesquioxide, yttrium oxide acceleration of sintering simultaneously, also create second phase particles at silicon carbide interface, promote to split Stricture of vagina deflects, and with the increase of second phase particles volume fraction, the fracture toughness of carborundum increases, its bending strength up to 586～ 650Mpa, fracture toughness is 7.15～7.40 Mpa.m1/2。
(2) in the manufacture method of the silicon nitride heat generating body of the present invention, with dehydrated alcohol (99. 9% purity) as medium, ball Mill mixing 24～72 hours, both ensure that batch mixing was uniform, had reduced again oxidative phenomena.Without appointing in the manufacturing process of the present invention What macromolecule modifier, and it is dependent on dry-pressing and isostatic cool pressing technique prepares the blank of high intensity.
(3) in the present invention, blank surface is uniformly coated with BN sealing coat, blank can be stoped to contact with the direct of graphite, disappear Possibility except high temperature case-carbonizing element.
(4) present invention is after hot pressed sintering, and the material stress of silicon nitride heat generating body is relatively big, at high temperature annealing 10～ It is slow cooling to room temperature after 24 hours, the stress of material can be eliminated.It addition, in high-temperature process, make the glass in material Glass crystallizes mutually, can eliminate the carbon of remnants further and reduce material stress.(the silicon nitride heating matrix of the present invention contains height Pure silicon nitride (Si3N4) powder body and a small amount of high-temperature liquid-phase sintering aid.Initial substrate raw material and heating wire are through dry-pressing and isostatic cool pressing Make blank, blank surface coating BN material.Blank hot pressed sintering at high temperature under high pressure becomes blank.Sintering blank high-temperature heat treatment Technique eliminates material stress and glass ceramics phase, has the feature of higher reliability and safety.
The microstructure under hot pressing condition of the silicon nitride heat generating body of inventive formulation and performance are as shown in the table:
Detailed description of the invention
Below in conjunction with embodiments of the invention, technical scheme is clearly and completely described.Obviously, Described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the reality in the present invention Execute example, all other embodiments that those of ordinary skill in the art are obtained under not making creative work premise, all belong to In the scope of protection of the invention.
Embodiment 1:
S1, choose the silicon nitride powder of 80 parts by weight, the aluminium sesquioxide powder of 0.1 parts by weight, three oxygen of 2 parts by weight Change two yttrium powders, the aluminium nitride powder of 3 parts by weight, the boron carbide powder of 1 parts by weight carry out proportioning mixing, by compound with High-temperature liquid-phase sintering aid inserts mixing in dehydrated alcohol by weight the ratio of 0.80:0.02, after batch mixing grinds 24 hours, through spray Formulation material is made in mist pelletize；
S1, by after dry-pressing formed for described formulation material, the most compressing by the isostatic cool pressing of 200MPa, and pressurize 5 minutes, To make blank；
S3, uniformly coat one layer of boron nitride sealing coat post-drying at described blank surface；
S4, blank is contained in hot pressing graphite jig then carries out hot pressed sintering, hot pressing graphite jig and the contact surface of blank are coated with There is one layer of described boron nitride sealing coat；Sintering pressure 20MPa, sintering temperature 1700 DEG C, temperature retention time 1 hour, to make hair Base；
S5, described blank is put in vacuum atmosphere oven, keep 1200 DEG C of constant temperature 24 hours, then naturally cool to room temperature.
Described boron nitride sealing coat is by thick with what dehydrated alcohol reconciled into after boron nitride powder and silicon nitride powder mixing Shape slurry；Wherein, silicon nitride powder with the part by weight of boron nitride powder is: 0.10:0.90.
Embodiment 2:
S1, choose the silicon nitride powder of 95 parts by weight, the aluminium sesquioxide powder of 5 parts by weight, three oxidations of 8 parts by weight Two yttrium powders, the aluminium nitride powder of 5 parts by weight, the boron carbide powder of 3 parts by weight carry out proportioning mixing, by compound with high Temperature liquid phase sintering inserts mixing in dehydrated alcohol by weight the ratio of 0.90:0.04, after batch mixing grinds 72 hours, through spraying Formulation material is made in pelletize；
S1, by after dry-pressing formed for described formulation material, the most compressing by the isostatic cool pressing of 250MPa, and pressurize 10 points Clock, to make blank；
S3, uniformly coat one layer of boron nitride sealing coat post-drying at described blank surface；
S4, blank is contained in hot pressing graphite jig then carries out hot pressed sintering, hot pressing graphite jig and the contact surface of blank are coated with There is one layer of described boron nitride sealing coat；Sintering pressure 50MPa, sintering temperature 1900 DEG C, temperature retention time 1 hour, to make hair Base；
S5, described blank is put in vacuum atmosphere oven, keep 1500 DEG C of constant temperature 10 hours, then naturally cool to room temperature.
Described boron nitride sealing coat is by thick with what dehydrated alcohol reconciled into after boron nitride powder and silicon nitride powder mixing Shape slurry；Wherein, silicon nitride powder with the part by weight of boron nitride powder is: 0.10:1.00.
Embodiment 3:
S1, choose the silicon nitride powder of 90 parts by weight, the aluminium sesquioxide powder of 3 parts by weight, three oxidations of 5 parts by weight Two yttrium powders, the aluminium nitride powder of 4 parts by weight, the boron carbide powder of 2 parts by weight carry out proportioning mixing, by compound with high Temperature liquid phase sintering inserts mixing in dehydrated alcohol by weight the ratio of 0.90:0.04, after batch mixing grinds 72 hours, through spraying Formulation material is made in pelletize；
S1, by after dry-pressing formed for described formulation material, the most compressing by the isostatic cool pressing of 220MPa, and pressurize 8 minutes, To make blank；
S3, uniformly coat one layer of boron nitride sealing coat post-drying at described blank surface；
S4, blank is contained in hot pressing graphite jig then carries out hot pressed sintering, hot pressing graphite jig and the contact surface of blank are coated with There is one layer of described boron nitride sealing coat；Sintering pressure 40MPa, sintering temperature 1900 DEG C, temperature retention time 4 hours, to make hair Base；
S5, described blank is put in vacuum atmosphere oven, keep 1400 DEG C of constant temperature 18 hours, then naturally cool to room temperature.
Described boron nitride sealing coat is by thick with what dehydrated alcohol reconciled into after boron nitride powder and silicon nitride powder mixing Shape slurry；Wherein, silicon nitride powder with the part by weight of boron nitride powder is: 0.10:0.95.
The microstructure under hot pressing condition of the silicon nitride heat generating body of above three embodiment and performance are as shown in the table:

Claims (6)

1. a silicon nitride heat generating body, it by pyrotoxin and heating body form, described pyrotoxin is tungsten filament, it is characterised in that: Described heating body is with silicon nitride (Si3N4), aluminium sesquioxide (A1203), yttrium oxide (Y203), aluminium nitride (A1N) be former Material, is formulated grinding, compression molding, high temperature sintering form, in terms of the gross weight of raw material, and the parts by weight of name component in raw material For:
Silicon nitride (Si3N4) 80～95
Aluminium sesquioxide (A1203) 0.1～5
Yttrium oxide (Y203) 2～8
Aluminium nitride (A1N) 3～5
Boron carbide (B4C) 1～3.
Silicon nitride heat generating body the most according to claim 1, it is characterised in that: in raw material, the parts by weight of name component are:
Silicon nitride (Si3N4) 90
Aluminium sesquioxide (A1203) 3
Yttrium oxide (Y203) 5
Aluminium nitride (A1N) 4
Boron carbide (B4C) 2.
3. the preparation method of a silicon nitride heat generating body as claimed in claim 1 or 2, it is characterised in that: the step of this preparation method Suddenly it is:
S1, by silicon nitride powder, aluminium sesquioxide powder, yttrium oxide powder, aluminium nitride powder, boron carbide powder by each Parts by weight carry out proportioning mixing, by compound and high-temperature liquid-phase sintering aid by weight 0.80～0.90:0.02～0.04 Ratio insert in dehydrated alcohol and mix, batch mixing ground after 24～72 hours, made formulation material through mist projection granulating；
S1, by after dry-pressing formed for described formulation material, the isostatic cool pressing by 200～250MPa is the most compressing, and pressurize 5 ～10 minutes, to make blank；
S3, uniformly coat one layer of boron nitride sealing coat post-drying at described blank surface；
S4, then carry out hot pressed sintering, sintering pressure 20～50MPa, sintering temperature 1700～1950 DEG C, temperature retention time 1～5 Hour, to make blank；
S5, described blank is put in vacuum atmosphere oven, keep 1200～1500 DEG C of constant temperature 10～24 hours, then natural cooling To room temperature.
Preparation method the most according to claim 3, it is characterised in that: described boron nitride sealing coat be by boron nitride powder and The thick shape slurry reconciled into dehydrated alcohol after silicon nitride powder mixing；Wherein, silicon nitride powder and the weight of boron nitride powder Ratio is: 0.10:0.90～1.00.
Preparation method the most according to claim 3, it is characterised in that: in described step 4, when carrying out hot pressed sintering, adopt Hot pressed sintering mould be hot pressing graphite jig.
Preparation method the most according to claim 3, it is characterised in that: use hot pressing graphite jig be hot pressed sintering mould Time, hot pressing graphite jig scribbles one layer of described boron nitride sealing coat on the contact surface of blank.
CN201510841326.1A 2015-11-28 2015-11-28 Silicon nitride heating element and preparation method thereof Pending CN105936595A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510841326.1A CN105936595A (en) 2015-11-28 2015-11-28 Silicon nitride heating element and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510841326.1A CN105936595A (en) 2015-11-28 2015-11-28 Silicon nitride heating element and preparation method thereof

Publications (1)

Publication Number Publication Date
CN105936595A true CN105936595A (en) 2016-09-14

Family

ID=57153070

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510841326.1A Pending CN105936595A (en) 2015-11-28 2015-11-28 Silicon nitride heating element and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105936595A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678530A (en) * 2019-01-24 2019-04-26 中国电子科技集团公司第四十三研究所 A kind of insulating powder and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1880280A (en) * 2005-06-13 2006-12-20 三和耐火工业股份有限公司 Refractory material comprising nanometer silicon carbide and its production method
CN102170716A (en) * 2010-12-09 2011-08-31 江苏华盛精细陶瓷科技有限公司 Method for manufacturing silicon nitride heating body
CN103096528A (en) * 2010-12-09 2013-05-08 江苏华盛精细陶瓷科技有限公司 Preparation method for silicon nitride heating body

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1880280A (en) * 2005-06-13 2006-12-20 三和耐火工业股份有限公司 Refractory material comprising nanometer silicon carbide and its production method
CN102170716A (en) * 2010-12-09 2011-08-31 江苏华盛精细陶瓷科技有限公司 Method for manufacturing silicon nitride heating body
CN103096528A (en) * 2010-12-09 2013-05-08 江苏华盛精细陶瓷科技有限公司 Preparation method for silicon nitride heating body

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678530A (en) * 2019-01-24 2019-04-26 中国电子科技集团公司第四十三研究所 A kind of insulating powder and preparation method thereof
CN109678530B (en) * 2019-01-24 2021-07-23 中国电子科技集团公司第四十三研究所 Isolation powder and preparation method thereof

Similar Documents

Publication Publication Date Title
CN104150940B (en) Silicon nitride and silicon carbide complex phase porous ceramics and preparation method thereof
CN103096529B (en) There is the manufacture method of the silicon nitride heat generating body of higher reliability and fail safe
CN101913879B (en) Silicon nitride material and preparation method thereof, as well as silicon nitride heating device and production method thereof
CN106904977B (en) Preparation of surface hard and core tough Si by two-step sintering method3N4Method for producing ceramic material
CN105236982B (en) The enhanced graphite-base composite material of aluminium nitride and preparation technology
CN113461426B (en) Compact high-hardness high-strength silicon nitride ceramic ball and preparation method and application thereof
CN106278283A (en) A kind of step sintering prepares the method for boron nitride ceramic material
CN101734923A (en) Aluminum nitride porous ceramic and preparation method thereof
CN109627014A (en) A kind of high-intensitive, high-termal conductivity Si3N4Ceramic material and preparation method thereof
CN103096528B (en) Preparation method for silicon nitride heating body
CN111943702A (en) In-situ synthesized beta-SIALON whisker toughened tungsten carbide composite material and preparation method and application thereof
CN101734920B (en) Titanium nitride porous ceramics and preparation method thereof
CN114524666A (en) High-strength dark-spot-free 95 aluminum oxide ceramic and preparation method thereof
CN103420677A (en) High strength and high oxidation resistance BN ceramic and preparation method thereof
CN104684870A (en) Silicon nitride sintered compact, heating device and adsorption device
CN105936595A (en) Silicon nitride heating element and preparation method thereof
CN112209722A (en) Silicon nitride composite material, preparation method thereof and heating element
CN114835473B (en) Alumina ceramic and preparation method thereof
CN109336614B (en) Preparation method of Sialon/Ti-22Al-25Nb ceramic matrix composite material
CN111196716A (en) Glaze-free heat-resistant daily white porcelain prepared from modified graphene and preparation process thereof
CN110877980A (en) High-strength silicon carbide/silicon nitride composite ceramic and preparation method thereof
CN107619282A (en) A kind of preparation method of high tenacity silicon titanium-carbide carborundum composite-phase ceramic shaped piece
CN106396664A (en) A magnesium-based lanthanum aluminate ceramic manufacturing method
CN107937790A (en) A kind of alumina-based ceramic metal material and preparation method thereof
JP5130599B2 (en) Method for producing hexagonal boron nitride sintered body and hexagonal boron nitride sintered body

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160914

RJ01 Rejection of invention patent application after publication