CN110143605A - A kind of preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON - Google Patents
A kind of preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON Download PDFInfo
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- CN110143605A CN110143605A CN201910595339.3A CN201910595339A CN110143605A CN 110143605 A CN110143605 A CN 110143605A CN 201910595339 A CN201910595339 A CN 201910595339A CN 110143605 A CN110143605 A CN 110143605A
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- dimensional
- sialon
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- energy consumption
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
-
- 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
- C04B41/5067—Silicon oxynitrides, e.g. SIALON
-
- 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
Abstract
The invention discloses the preparation methods of diamond surface low energy consumption synthesizing one-dimensional SiAlON a kind of, and the preparation method comprises the following steps, and silicon powder and bortz powder according to proper proportion uniform stirring and are subject to compound binding agent and mixed by (1)；(2) mixed powder is pressed into high porosity regular shape prefabricated blank；(3) prefabricated blank is dried, is put into togerther in tube furnace and heats with aluminium block；(4) it is communicated in furnace with atmosphere, normal pressure heat-insulating, after cooling, diamond surface prepares one-dimensional SiAlON.The present invention utilizes nitridation reaction method and CRN method synthesizing one-dimensional SiAlON, synthesizes the one-dimensional SiAlON of high-purity with low cost, low energy consumption.
Description
Technical field
The present invention relates to the preparation method technical fields of one-dimensional SiAlON, and in particular to a kind of diamond surface low energy consumption conjunction
At the preparation method of one-dimensional SiAlON.
Background technique
SiAlON material is made pottery with its excellent chemical stability, unique high-temperature comprehensive property in high-quality fine structure
It is widely used in porcelain and advanced refractory material, distinctive mono-crystalline structures are even more to impart good mechanical property, optical
Energy and electric property, make SiAlON material be provided with more wide application prospect in fields such as optics, electricity, refractory ceramics.
The essence of SiAlON material is Si3N4In Si and N atom the solid solution to be formed, researcher are replaced by Al and O respectively
At present mainly for prepare different-shape SiAlON material and reduce cost of material researched and analysed.Nowadays SiAlON material
Main preparation methods have solid reaction process, Self- propagating Sintering Synthetic method, CRN method.SiAlON material is to synthesis temperature
Degree is quite sensitive, the excessively high or too low progress for being all unfavorable for reaction, reports most preparation temperature at present at 1400 DEG C -1700
Between DEG C, preparation temperature is required to remain high, reduces high energy consumption in preparation SiAlON materials process and be still current researcher
Emphasis direction.In preparation SiAlON materials process, it to be constantly passed through high pure nitrogen, preparation requires strictly, to improve
Cost of material.As production technology is continuously improved in diamond, cost of material is constantly reduced, and industrial silica fume is cheap, is
The following low cost, low energy consumption, low requirement synthesis SiAlON material provide a kind of completely new synthetic method.
Summary of the invention
Problem to be solved by this invention is: providing the preparation side of diamond surface low energy consumption synthesizing one-dimensional SiAlON a kind of
Method, it is one-dimensional with low cost, low energy consumption synthesis high-purity using nitridation reaction method and CRN method synthesizing one-dimensional SiAlON
SiAlON。
The present invention in order to solve the above problem provided by technical solution are as follows: a kind of diamond surface low energy consumption synthesizing one-dimensional
The preparation method of SiAlON, the preparation method comprises the following steps,
(1) silicon powder and bortz powder according to proper proportion uniform stirring and are subject to compound binding agent and mixed；
(2) mixed powder is pressed into high porosity regular shape prefabricated blank；
(3) prefabricated blank is dried, is put into togerther in tube furnace and heats with aluminium block；
(4) it is communicated in furnace with atmosphere, normal pressure heat-insulating, after cooling, diamond surface prepares one-dimensional SiAlON.
Preferably, the weight percent of the bortz powder in the step (1) and silicon powder is respectively bortz powder 20%-
50%, silicon powder 10%-50%, used diamond are that monocrystalline or diamond are crushed powder, diamond particles specification 50-
200 mesh, silicon powder specification 100-500 mesh.
Preferably, the compound binding agent in the step (1) is polyvinyl alcohol and dehydrated alcohol.
Preferably, press temperature is room temperature, pressing pressure 2MPa-15MPa in the step (2).
Preferably, tube furnace is directly connect with atmosphere in the step (4), without being passed through gas in any form.
Preferably, the temperature of the drying process of the step (3) is 50 DEG C -100 DEG C, drying time 30min-
120min。
Preferably, furnace inner gas pressure is 0MPa in the step (4), at 900 DEG C -1200 DEG C, keeps the temperature 120min-
300min。
Preferably, aluminium block is rafifinal, with the green body of aluminium powder compacting, silumin in the step (3).
Compared with prior art, the invention has the advantages that
(1) raw material use diamond and technical grade silicon powder, low in cost.
(2) it directly reacts inside billet surface and green body, reduces experiment link, improve synthesizing one-dimensional
The combined coefficient of SiAlON.
(3) low energy consumption in preparation process, temperature control is at 1300 DEG C hereinafter, not needing to be passed through high pure nitrogen, whole and sky
Gas connection, greatly reduces the requirement of production cost and preparation process to equipment.
(4) Si can be utilized with high degree3N4, improve one-dimensional SiAlON degree of purity.
(5) preparation process is pollution-free.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.
Fig. 1 is that SiAlON is compared in diamond different orientation face pattern.
Fig. 2 is the microscopic appearance under SiAlON whisker SEM.
Fig. 3 is SiAlON in diamond particle surfaces growth conditions.
Fig. 4 is the XRD spectrum of diamond Si AlON.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with accompanying drawings and embodiments, how the present invention is applied whereby
Technological means solves technical problem and reaches the realization process of technical effect to fully understand and implement.
Embodiment 1
It weighs 2 gram of 200 mesh diamond particles respectively and 2 gram of 200 mesh technical grade silicon powder is subject to compound binding agent and uniformly mixes
Mixed powder is put into the mold of 10 φ and is suppressed with the pressure of 5MPa by stirring, and pressure maintaining is taken out after two minutes, obtains green body.Then
Green body is dried with the technique of 50 DEG C of temperature 30min, green body and high-purity aluminium block with oxidation film are put in pipe
Preparation process is carried out in formula furnace, is heated to 1000 DEG C of heat preservation 3h, wherein sample preparation whole process is contacted with atmosphere, sample furnace cooling
Afterwards, diamond surface synthesizes one-dimensional SiAlON.
Embodiment 2
It weighs 2 gram of 200 mesh diamond particles respectively and 2 gram of 200 mesh technical grade silicon powder is subject to compound binding agent and uniformly mixes
Mixed powder is put into the mold of 10 φ and is suppressed with the pressure of 10MPa by stirring, and pressure maintaining is taken out after two minutes, obtains green body.Then
Green body is dried with the technique of 70 DEG C of temperature 60min, green body and high-purity aluminium block with oxidation film are put in pipe
Preparation process is carried out in formula furnace, is heated to 1100 DEG C of heat preservation 4h, wherein sample preparation whole process is contacted with atmosphere, sample furnace cooling
Afterwards, diamond surface synthesizes one-dimensional SiAlON.
Embodiment 3
It weighs 2 gram of 200 mesh diamond particles respectively and 2 gram of 200 mesh technical grade silicon powder is subject to compound binding agent and uniformly mixes
Mixed powder is put into the mold of 10 φ and is suppressed with the pressure of 15MPa by stirring, and pressure maintaining is taken out after two minutes, obtains green body.Then
Green body is dried with the technique of 80 DEG C of temperature 120min, green body and high-purity aluminium block with oxidation film are put in pipe
Preparation process is carried out in formula furnace, is heated to 1300 DEG C of heat preservation 4h, wherein sample preparation whole process is contacted with atmosphere, sample furnace cooling
Afterwards, diamond surface synthesizes one-dimensional SiAlON.
The present invention using nitridation reaction method and CRN method in diamond surface low energy consumption synthesizing one-dimensional SiAlON,
Skimming processes occur for compound binding agent, and silicon powder comes into full contact with diamond particles and reacts, equal in diamond different orientation face
Synthesizing silicon carbide coating, in gas-solid interface, anti-life is anti-with the nitrogen in air first for a part of silicon powder directly contacted with aluminium block
It answers, forms the Si of one layer of tight silicon powder3N4Layer, Si3N4Layer and the oxidation film on aluminium block surface react to form AlN, the life
Facilitate Al at object2O3To Si3N4It is spread in layer, forms SiAlON phase.When molten aluminum is melted, green body is entered by capillary force
Inside, a part of diamond particles are carbonized, and nitridation reaction and carbon thermal reduction occur for nitrogen in molten aluminum and SiC coating and air
Nitridation reaction, in diamond surface synthesizing one-dimensional SiAlON.
Only highly preferred embodiment of the present invention is described above, but is not to be construed as limiting the scope of the invention.This
Invention is not only limited to above embodiments, and specific structure is allowed to vary.All protection models in independent claims of the present invention
Interior made various change is enclosed to all fall in the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON, it is characterised in that: the preparation method packet
Include following steps,
(1) silicon powder and bortz powder according to proper proportion uniform stirring and are subject to compound binding agent and mixed；
(2) mixed powder is pressed into high porosity regular shape prefabricated blank；
(3) prefabricated blank is dried, is put into togerther in tube furnace and heats with aluminium block；
(4) it is communicated in furnace with atmosphere, normal pressure heat-insulating, after cooling, diamond surface prepares one-dimensional SiAlON.
2. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: the weight percent of bortz powder and silicon powder in the step (1) is respectively bortz powder 20%-50%, silicon powder
10%-50%, used diamond are that monocrystalline or diamond are crushed powder, diamond particles specification 50-200 mesh, silicon powder
Specification 100-500 mesh.
3. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: the compound binding agent in the step (1) is polyvinyl alcohol and dehydrated alcohol.
4. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: press temperature is room temperature, pressing pressure 2MPa-15MPa in the step (2).
5. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: tube furnace is directly connect with atmosphere in the step (4), without being passed through gas in any form.
6. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: the temperature of the drying process of the step (3) is 50 DEG C -100 DEG C, drying time 30min-120min.
7. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: furnace inner gas pressure is 0MPa in the step (4), at 900 DEG C -1200 DEG C, keeps the temperature 120min-300min.
8. the preparation method of diamond surface low energy consumption synthesizing one-dimensional SiAlON according to claim 1 a kind of, feature
Be: aluminium block is rafifinal, with the green body of aluminium powder compacting, silumin in the step (3).
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Citations (7)
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|---|---|---|---|---|
| US4528244A (en) * | 1983-09-30 | 1985-07-09 | Dresser Industries, Inc. | Fused silica shapes |
| US5601874A (en) * | 1994-12-08 | 1997-02-11 | The Dow Chemical Company | Method of making moisture resistant aluminum nitride powder and powder produced thereby |
| CN1919792A (en) * | 2006-09-04 | 2007-02-28 | 青岛大学 | Manufacture method of silicon carbide refractory ceramics material |
| CN100999412A (en) * | 2006-12-14 | 2007-07-18 | 哈尔滨工业大学（威海） | Sialon quasi monodimension nanometer material and its preparation method |
| CN102701745A (en) * | 2012-05-23 | 2012-10-03 | 合肥工业大学 | Synthesis method of submicron claviform beta-Sialon |
| JP2017160102A (en) * | 2016-03-11 | 2017-09-14 | 一般財団法人ファインセラミックスセンター | Environment resistant coating member |
| CN108610067A (en) * | 2018-05-18 | 2018-10-02 | 中钢集团耐火材料有限公司 | A kind of silicon carbide articles and preparation method thereof of Gao Sailong phases |
-
2019
- 2019-07-03 CN CN201910595339.3A patent/CN110143605A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528244A (en) * | 1983-09-30 | 1985-07-09 | Dresser Industries, Inc. | Fused silica shapes |
| US5601874A (en) * | 1994-12-08 | 1997-02-11 | The Dow Chemical Company | Method of making moisture resistant aluminum nitride powder and powder produced thereby |
| CN1919792A (en) * | 2006-09-04 | 2007-02-28 | 青岛大学 | Manufacture method of silicon carbide refractory ceramics material |
| CN100999412A (en) * | 2006-12-14 | 2007-07-18 | 哈尔滨工业大学（威海） | Sialon quasi monodimension nanometer material and its preparation method |
| CN102701745A (en) * | 2012-05-23 | 2012-10-03 | 合肥工业大学 | Synthesis method of submicron claviform beta-Sialon |
| JP2017160102A (en) * | 2016-03-11 | 2017-09-14 | 一般財団法人ファインセラミックスセンター | Environment resistant coating member |
| CN108610067A (en) * | 2018-05-18 | 2018-10-02 | 中钢集团耐火材料有限公司 | A kind of silicon carbide articles and preparation method thereof of Gao Sailong phases |
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Application publication date: 20190820 |