CN107867862A - A kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis and preparation method thereof - Google Patents

A kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis and preparation method thereof Download PDF

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CN107867862A
CN107867862A CN201610845973.4A CN201610845973A CN107867862A CN 107867862 A CN107867862 A CN 107867862A CN 201610845973 A CN201610845973 A CN 201610845973A CN 107867862 A CN107867862 A CN 107867862A
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powder
ceramic balls
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徐常明
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Suzhou Portsmouth Mstar Technology Ltd
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Abstract

The present invention relates to Ceramic Balls of a kind of reaction in-situ pressureless sintering synthesis and preparation method thereof.It is an advantage of the invention that：Technique is simple, cost is low.The present invention is densified using magnesium-yttrium-transition metal powder, boron carbide powder as raw material by reaction in-situ in 1,700 2300 DEG C of pressureless sinterings, and reaction is carried out simultaneously with densification.The MB sintered2MC Ceramic Balls are by MB2, the phase compositions of MC two.Relative to two phase ceramics are first synthesized, sintering is remixed, technological process is become simple；Mechanical property is good.Because two-phase is by in-situ reactive synthesis, there is good interfacing relationship, so as to improve the mechanical property of composite.

Description

A kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis and preparation method thereof
Technical field
The present invention relates to Ceramic Balls and preparation method, the Ceramic Balls of specially a kind of reaction in-situ pressureless sintering synthesis and its Preparation method.
Background technology
MB2It is the compound of hexagonal crystal system C32 type structures（M is titanium, zirconium, hafnium, vanadium, niobium, tantalum）, it has a series of excellent Physical and chemical properties：High-melting-point (3000 more than K), high rigidity, high elastic modulus, good chemical stability, electrical conductance And thermal conductance.These excellent physical and chemical properties cause MB2High-performance ceramic ball material can be used as.In addition, MC chemical combination Thing also has high rigidity, high elastic modulus, good chemical stability, and the mechanical property of Ceramic Balls can be mutually improved as enhancing Energy.Using magnesium-yttrium-transition metal titanium, zirconium, hafnium, vanadium, niobium, tantalum and boron carbide powder as raw material, using magnesium-yttrium-transition metal and boron carbide in high temperature Under reaction, in-situ preparation MB2And MC, MB is prepared using hot-press method in previous studies2- MC composites（Metal. Mater. Trans. A, 39（2008）1496-1505）Succeed.So far, there has been no MB2- MC composites Ceramic Balls pressureless sintering is successfully prepared and applied, therefore the present invention has very strong novelty.
In sample preparation, we use reaction in-situ pressureless sintering synthetic technology, and its principle is to match somebody with somebody raw material on request Than making it that chemical reaction generation target product occur in high temperature, while the material of densification is obtained with from sintering process.Its advantage Be technique is simple, time saving province can, product fabricated in situ.
The content of the invention
It is in situ it is an object of the invention to design the low one kind of a kind of good mechanical property, easy control of process conditions, cost Ceramic Balls of pressureless sintering synthesis and preparation method thereof are reacted, the technical solution adopted for the present invention to solve the technical problems is： A kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis, it is characterised in that：The component of the Ceramic Balls is MB2- MC, wherein, M is Magnesium-yttrium-transition metal Ti, Zr, Hf, V, Nb or Ta；Form the twenty percent split-phase MB of Ceramic Balls2Generated with MC by reaction in-situ；Group Into the MB of Ceramic Balls2Mol ratio with MC twenty percent split-phases is 2:1.
The preparation method of the Ceramic Balls, its step are：
（1）, first, using the Ti powder in magnesium-yttrium-transition metal powder, Zr powder, Hf powder, V powder, Nb powder or Ta powder and boron carbide powder as Raw material, the mol ratio between magnesium-yttrium-transition metal powder and boron carbide powder are 3：1, using absolute alcohol as medium the ball milling in agate pot 16-30 hours；
（2）, then, drying mixed powder simultaneously sieve, powder is fitted into isostatic cool pressing balling-up in rubber mold, isostatic cool pressing process is adopted Pressure is 100-300 MPa；
（3）, it is last, sintered in vacuum or be connected with the graphite furnace of argon gas, the heating rate used is per minute for 1-30 DEG C, burning Junction temperature is 1700-2300 DEG C, and soaking time is 1-4 hours；
（4）, the ceramic ball warp obtained through oversintering is successively by rough polishing, 9 micron diamond polishing fluid tumblings, 3 micron chickens After the tumbling of hard rock polishing fluid, 1 micron diamond polishing fluid tumbling, the Ceramic Balls of high-precision size are obtained.
The preferable step（1）The Ti powder of middle addition, Zr powder, Hf powder, V powder, Nb powder or Ta powder and boron carbide powder Particle size range is 200~10000 mesh.
The preferable step（1）Raw material in can add sintering aid.
The diameter range of the preferable Ceramic Balls prepared is 1-30 millimeters.
It is an advantage of the invention that：
1. technique is simple, cost is low.The present invention is existed using magnesium-yttrium-transition metal powder, boron carbide powder as raw material by reaction in-situ 1700-2300 DEG C of pressureless sintering densification, reaction are carried out simultaneously with densification.The MB sintered2- MC Ceramic Balls are by MB2, MC two Phase composition（A small amount of additive or enhancing phase can be added）.Relative to two phase ceramics are first synthesized, sintering is remixed, makes technique stream Journey becomes simple.
2. mechanical property is good, because two-phase is by in-situ reactive synthesis, there is good interfacing relationship, it is compound so as to improve The mechanical property of material.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is ZrB in the specific embodiment of the invention one2The X-ray diffraction phase composition analysis of-ZrC Ceramic Balls；
Fig. 2 is ZrB in the specific embodiment of the invention one2The fracture apperance of-ZrC Ceramic Balls（Secondary electron image）.
Embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.Accompanying drawing is simplified schematic diagram, only with signal side Formula illustrates the basic structure of the present invention, therefore it only shows the composition relevant with the present invention.
Specific embodiment one, a kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis, it is characterised in that：The Ceramic Balls Component is MB2- MC, wherein, M is magnesium-yttrium-transition metal Zr；Form the twenty percent split-phase ZrB of Ceramic Balls2Generated with ZrC by reaction in-situ； Form the ZrB of Ceramic Balls2Mol ratio with ZrC twenty percent split-phases is 2:1.
The preparation method of the Ceramic Balls, its step are：
（1）, first, using the Zr powder in magnesium-yttrium-transition metal powder and boron carbide powder as raw material, magnesium-yttrium-transition metal powder Zr powder and boron carbide Mol ratio between powder is 3：1, using absolute alcohol as medium ball milling 25 hours in agate pot；
（2）, then, drying mixed powder simultaneously sieve, powder is fitted into isostatic cool pressing balling-up in rubber mold, isostatic cool pressing process is adopted Pressure is 200 MPa；
（3）, it is last, sintered in the graphite furnace for be connected with argon gas, the heating rate used is per minute for 6 DEG C, and sintering temperature is 1900 DEG C, soaking time is 2.5 hours；
（4）, the ceramic ball warp obtained through oversintering is successively by rough polishing, 9 micron diamond polishing fluid tumblings, 3 micron chickens After the tumbling of hard rock polishing fluid, 1 micron diamond polishing fluid tumbling, the Ceramic Balls of high-precision size are obtained.
The step（1）The Zr powder and boron carbide powder particle size range of middle addition are 200~10000 mesh.
The step（1）Raw material in can add sintering aid.
The diameter range of the Ceramic Balls prepared is 1-30 millimeters.
As can be seen from Figure 1 the main component in sample is mutually ZrB2And ZrC, contain a small amount of zirconium oxide.Zirconium oxide May be the introducing generation of a small amount of oxygen in sintering process, its presence can promote the sintering densification of ceramics.
Figure it is seen that zirconium diboride crystal grain mainly shows tabular crystalline form state, zirconium carbide crystal grain is isometric particle. Prepared sample airtight air vent is seldom, shows that sample has very high consistency.
Specific embodiment two, a kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis, it is characterised in that：The Ceramic Balls Component is MB2- MC, wherein, M is magnesium-yttrium-transition metal Ti；Form the twenty percent split-phase TiB of Ceramic Balls2Generated with TiC by reaction in-situ； Form the TiB of Ceramic Balls2Mol ratio with TiC twenty percent split-phases is 2:1.
The preparation method of the Ceramic Balls, its step are：
（1）, first, using the Ti powder in magnesium-yttrium-transition metal powder and boron carbide powder as raw material, magnesium-yttrium-transition metal powder Ti powder and boron carbide Mol ratio between powder is 3：1, using absolute alcohol as medium ball milling 16 hours in agate pot；
（2）, then, drying mixed powder simultaneously sieve, powder is fitted into isostatic cool pressing balling-up in rubber mold, isostatic cool pressing process is adopted Pressure is 100 MPa；
（3）, it is last, sintered in the graphite furnace of vacuum, the heating rate used is per minute for 1 DEG C, sintering temperature 1700 DEG C, soaking time is 4 hours；
（4）, the ceramic ball warp obtained through oversintering is successively by rough polishing, 9 micron diamond polishing fluid tumblings, 3 micron chickens After the tumbling of hard rock polishing fluid, 1 micron diamond polishing fluid tumbling, the Ceramic Balls of high-precision size are obtained.
The step（1）The Ti powder and boron carbide powder particle size range of middle addition are 200~10000 mesh.
The step（1）Raw material in can add sintering aid.
The diameter range of the Ceramic Balls prepared is 1-30 millimeters.
Products therefrom composition is ferro-boron pure phase as can see from Figure 1, and gained powdery pulp is with sharp as can see from Figure 2 The size distribution curve of light bead degree sedimentometer test.
Specific embodiment three, a kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis, it is characterised in that：The Ceramic Balls Component is MB2- MC, wherein, M is magnesium-yttrium-transition metal V；Form the twenty percent split-phase VB of Ceramic Balls2Generated with VC by reaction in-situ；Group Into the VB of Ceramic Balls2Mol ratio with VC twenty percent split-phases is 2:1.
The preparation method of the Ceramic Balls, its step are：
（1）, first, using the V powder in magnesium-yttrium-transition metal powder and boron carbide powder as raw material, magnesium-yttrium-transition metal powder V powder and boron carbide powder Between mol ratio be 3：1, using absolute alcohol as medium ball milling 30 hours in agate pot；
（2）, then, drying mixed powder simultaneously sieve, powder is fitted into isostatic cool pressing balling-up in rubber mold, isostatic cool pressing process is adopted Pressure is 300 MPa；
（3）, it is last, sintered in the graphite furnace for be connected with argon gas, the heating rate used is per minute for 30 DEG C, and sintering temperature is 2000 DEG C, soaking time is 1 hour；
（4）, the ceramic ball warp obtained through oversintering is successively by rough polishing, 9 micron diamond polishing fluid tumblings, 3 micron chickens After the tumbling of hard rock polishing fluid, 1 micron diamond polishing fluid tumbling, the Ceramic Balls of high-precision size are obtained.
The step（1）The V powder and boron carbide powder particle size range of middle addition are 200~10000 mesh.
The step（1）Raw material in can add sintering aid.
The diameter range of the Ceramic Balls prepared is 1-30 millimeters..
It is an advantage of the invention that：
1. technique is simple, cost is low.The present invention is existed using magnesium-yttrium-transition metal powder, boron carbide powder as raw material by reaction in-situ 1700-2300 DEG C of pressureless sintering densification, reaction are carried out simultaneously with densification.The MB sintered2- MC Ceramic Balls are by MB2, MC two Phase composition（A small amount of additive or enhancing phase can be added）.Relative to two phase ceramics are first synthesized, sintering is remixed, makes technique stream Journey becomes simple.
2. mechanical property is good.Because two-phase is by in-situ reactive synthesis, there is good interfacing relationship, it is compound so as to improve The mechanical property of material.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to this patent as enlightenment Various changes and amendments can be carried out in the range of without departing from this item patented technology thought entirely.The technology of this item patent Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.

Claims (5)

  1. A kind of 1. Ceramic Balls of reaction in-situ pressureless sintering synthesis, it is characterised in that：The component of the Ceramic Balls is MB2- MC, its In, M is magnesium-yttrium-transition metal Ti, Zr, Hf, V, Nb or Ta；Form the twenty percent split-phase MB of Ceramic Balls2With MC by reaction in-situ Generation；Form the MB of Ceramic Balls2Mol ratio with MC twenty percent split-phases is 2:1.
  2. 2. according to the preparation method of Ceramic Balls described in claim 1, it is characterised in that its step is：
    （1）, first, using the Ti powder in magnesium-yttrium-transition metal powder, Zr powder, Hf powder, V powder, Nb powder or Ta powder and boron carbide powder as Raw material, the mol ratio between magnesium-yttrium-transition metal powder and boron carbide powder are 3：1, using absolute alcohol as medium the ball milling in agate pot 16-30 hours；
    （2）, then, drying mixed powder simultaneously sieve, powder is fitted into isostatic cool pressing balling-up in rubber mold, isostatic cool pressing process is adopted Pressure is 100-300 MPa；
    （3）, it is last, sintered in vacuum or be connected with the graphite furnace of argon gas, the heating rate used is per minute for 1-30 DEG C, burning Junction temperature is 1700-2300 DEG C, and soaking time is 1-4 hours；
    （4）, through oversintering obtain ceramic ball warp successively by rough polishing, 9 micron diamond polishing fluid tumblings, 3 micron chickens After the tumbling of hard rock polishing fluid, 1 micron diamond polishing fluid tumbling, the Ceramic Balls of high-precision size are obtained.
  3. 3. according to the preparation method of the Ceramic Balls described in claim 2, it is characterised in that：The step（1）The Ti powder of middle addition, Zr powder, Hf powder, V powder, Nb powder or Ta powder and boron carbide powder particle size range are 200~10000 mesh.
  4. 4. according to the preparation method of the Ceramic Balls described in claim 2, it is characterised in that：The step（1）Raw material in can be with Add sintering aid.
  5. 5. according to the preparation method of the Ceramic Balls described in claim 2, it is characterised in that：The diameter of the Ceramic Balls prepared Scope is 1-30 millimeters.
CN201610845973.4A 2016-09-25 2016-09-25 A kind of Ceramic Balls of reaction in-situ pressureless sintering synthesis and preparation method thereof Pending CN107867862A (en)

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US5720910A (en) * 1995-07-26 1998-02-24 Vlajic; Milan D. Process for the production of dense boron carbide and transition metal carbides
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