CN102491754A - Preparation method for compact ultrahigh temperature multi-layer ceramic material - Google Patents
Preparation method for compact ultrahigh temperature multi-layer ceramic material Download PDFInfo
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- CN102491754A CN102491754A CN2011103827582A CN201110382758A CN102491754A CN 102491754 A CN102491754 A CN 102491754A CN 2011103827582 A CN2011103827582 A CN 2011103827582A CN 201110382758 A CN201110382758 A CN 201110382758A CN 102491754 A CN102491754 A CN 102491754A
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Abstract
The present invention relates to a preparation method for a compact ultrahigh temperature multi-layer ceramic material. The technical scheme of the present invention is characterized in that powder materials of ZrB2 and SiC are adopted as main raw materials, and a certain additive is adopted to prepare a casting slurry with good stability and good fluidity; the casting slurry is subjected to vacuum defoaming and casting drying to obtain a bisque; the prepared ZrB2 phase bisque sheets and the prepared SiC phase bisque sheets are alternately layered, clipped and aligned; the aligned sheets are filled in a graphite mold, and are subjected to cold isostatic pressing pre-forming and glue discharging; finally a hot pressing sintering treatment is performed for 2 hours respectively at temperatures of 1900 DEG C, 1950 DEG C and 2000 DEG C under pressure of 35 MPa in the protection of Ar atmosphere, wherein the densities at different sintering temperatures are respectively 97.7%, 99.7% and 99.1% with validations, and the whole density of the laminated ceramic material in the prior art is difficultly achieved due to the interlayer sintering anisotropy. In addition, the bisque sheets of the present invention are prepared by the water-base casting method, no pollution is generated, the design of the laminated structure has the pluralism characteristic, and the important characteristic of the present invention is simple components and complex structure.
Description
Technical field
The present invention relates to a kind of fine and close ultrahigh-temperature multilayer ceramic preparation methods, problems such as the preparation material technology that exists in prior art complicacy, density refractory breakthrough.
Background technology
Gliding type strategic maneuver bullet when supersonic vehicle, long boat, superelevation velocity of sound reentry vehicle sharp-pointed leading edge or housing when extreme pneumatic heating condition flight may cause passivation owing to ablation; This will reduce other performances such as speed of guided missile and aircraft, must adopt suitable material and appropriate means to produce and satisfy the ultrahigh-temperature assembly that non-ablation requires.As anti-ablation hyperthermal material, its compactness requires very high, and the structure design of material needs complicated flexibly.
Superhigh temperature ceramic material, the especially boride of refractory metal Zr, Hf and Ta, carbide have represented working temperature at the feasible candidate material more than 2000 ℃.These materials have important use at space industry and are worth, thereby receive great concern.
The preparation technology of superhigh temperature ceramic material mainly is hot pressed sintering and discharge plasma sintering at present; But these technologies do not have big progress aspect optimization; And make the high stupalith of compactness and only limit to block body ceramic material; Difficulty satisfies the requirement of material structure design complexity, and the material of gained also only limits to preparation and performance study in the laboratory.Ceramic layered material will cause densification rate inconsistent because the sintering anisotropy between existence layer and the layer can show different sintering behaviors thus, be difficult to the densification that reaches whole.
Summary of the invention
The technical problem that solves
For fear of the weak point of prior art, the present invention proposes a kind of fine and close ultrahigh-temperature multilayer ceramic preparation methods, is a kind of pollution-free, and can satisfy the requirement of material structure design diversification, the most important high hyperthermal material of compactness that makes.
Technical scheme
A kind of fine and close ultrahigh-temperature multilayer ceramic preparation methods is characterized in that step is following:
Step 1: with ZrB
2, 20～40vol% SiC and less than the B of 10vol%
4Carry out ball milling in C adding 50～60vol% zero(ppm) water and the 1.9～2vol% dispersion agent TMAH; The sticker PVA solution and the 6～7vol% softening agent 1 that add 20～30vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 500～1000 μ m, behind the knifing at air drying and be prepared into A laminin base; The concentration of said PVA solution is 5%; Above-mentioned each percent by volume is for accounting for ZrB
2The percent by volume of powder volume;
Step 2: with the B of SiC and 5vol%
4Carry out ball milling in C adding 50～60vol% zero(ppm) water and the 0.6～0.7vol% dispersion agent TMAH; The sticker PVA solution and the 6～7vol% softening agent 1 that add 20～30vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 500～1000 μ m, behind the knifing at air drying and be prepared into B laminin base; Above-mentioned each percent by volume is the percent by volume that accounts for SiC powder volume;
Step 3: with A laminin base and the B laminin base alternative stacked after the cutting that requires according to sample, through isostatic cool pressing premolding, pressure is 189MPa, dwell time 60s, one-level release time 30s, secondary release time 8s;
Step 4: place graphite jig to be incubated 1 hour down at 500 ℃ and carry out binder removal, carry out hot pressed sintering then, the agglomerating condition is: sintering range is incubated 2 hours at 1850 ℃～2000 ℃, and pressure is about 35MPa, and atmosphere is Ar.
Alternative stacked in the step 3 is a multilayer.
The multilayer of alternative stacked is A layer and B layer crossing stack.
The multilayer of alternative stacked is a plurality of A layers and a plurality of B layer crossing stack.
Beneficial effect
A kind of fine and close ultrahigh-temperature multilayer ceramic preparation methods that the present invention proposes, beneficial effect is: (1) replaces organic curtain coating legal system to get uniform and stable slurry with water base casting process, and is pollution-free; (2) preparation technology is flexible, can carry out the design of big specification sample and complex construction sample, and density is high.The present invention effectively solves sample density problem, for the complex construction goods provide the preparation possibility.
Description of drawings
Fig. 1: the mould southwest normal axomometric drawing of self-control tape casting diaphragm;
Fig. 2: SEM figure in square section behind the ultrahigh-temperature multilayer ceramic sample sintering;
Fig. 3: the SEM figure of junction between ultrahigh-temperature multilayer ceramic two phases;
Embodiment
Combine embodiment, accompanying drawing that the present invention is further described at present:
Instance one:
(1) with ZrB
2+ 20vol%SiC+5vol%B
4Carry out ball milling in C adding 50vol% zero(ppm) water and the 1.95vol% dispersion agent TMAH; The sticker PVA solution and the 6.35vol% softening agent 1 that add 25vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 800 μ m, behind the knifing at air drying and be prepared into A laminin base; The concentration of said PVA solution is 5%;
Step 2: with SiC+5vol%B
4Carry out ball milling in C adding 55vol% zero(ppm) water and the 0.65vol% dispersion agent TMAH; The sticker PVA solution and the 6.35vol% softening agent 1 that add 25vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 800 μ m, behind the knifing at air drying and be prepared into B laminin base;
Step 3: with A laminin base and the B laminin base alternative stacked after the cutting that requires according to sample, through isostatic cool pressing premolding, pressure is 189MPa, dwell time 60s, one-level release time 30s, secondary release time 8s;
Step 4: place graphite jig to be incubated 1 hour down at 500 ℃ and carry out binder removal, carry out hot pressed sintering then, the agglomerating condition is: sintering temperature is 1850 ℃, is incubated 2 hours, and pressure is about 35MPa, and atmosphere is Ar.
Alternative stacked in the step 3 is a multilayer.
The multilayer of alternative stacked is A layer and B layer crossing stack.
The multilayer of alternative stacked is a plurality of A layers and a plurality of B layer crossing stack (A+B+A+B...).
Instance two:
1) with ZrB
2+ 36vol%SiC+5vol%B
4Carry out ball milling in C adding 55vol% zero(ppm) water and the 1.95vol% dispersion agent TMAH; The sticker PVA solution and the 6.35vol% softening agent 1 that add 25vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 600 μ m, behind the knifing at air drying and be prepared into A laminin base; The concentration of said PVA solution is 5%;
Step 2: with SiC+5vol%B
4Carry out ball milling in C adding 55vol% zero(ppm) water and the 0.65vol% dispersion agent TMAH; The sticker PVA solution and the 6.35vol% softening agent 1 that add 25vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 600 μ m, behind the knifing at air drying and be prepared into B laminin base;
Step 3: with A laminin base and the B laminin base alternative stacked after the cutting that requires according to sample, through isostatic cool pressing premolding, pressure is 189MPa, dwell time 60s, one-level release time 30s, secondary release time 8s;
Step 4: place graphite jig to be incubated 1 hour down at 500 ℃ and carry out binder removal, carry out hot pressed sintering then, the agglomerating condition is: sintering range is incubated 2 hours at 1900 ℃, and pressure is about 35MPa, and atmosphere is Ar.
Alternative stacked in the step 3 is a multilayer.
The multilayer of alternative stacked is two A layers and B layer crossing stack.
The multilayer of alternative stacked is a plurality of A layers and a plurality of B layer crossing stack (A+A+B+A+A+B...).
Instance three:
1) with ZrB
2+ 40vol%SiC+5vol%B
4Carry out ball milling in C adding 60vol% zero(ppm) water and the 1.95vol% dispersion agent TMAH; The sticker PVA solution and the 6.35vol% softening agent 1 that add 25vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 500 μ m, behind the knifing at air drying and be prepared into A laminin base; The concentration of said PVA solution is 5%;
Step 2: with SiC+5vol%B
4Carry out ball milling in C adding 55vol% zero(ppm) water and the 0.65vol% dispersion agent TMAH; The sticker PVA solution and the 6.35vol% softening agent 1 that add 25vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 500 μ m, behind the knifing at air drying and be prepared into B laminin base;
Step 3: with A laminin base and the B laminin base alternative stacked after the cutting that requires according to sample, through isostatic cool pressing premolding, pressure is 189MPa, dwell time 60s, one-level release time 30s, secondary release time 8s;
Step 4: place graphite jig to be incubated 1 hour down at 500 ℃ and carry out binder removal, carry out hot pressed sintering then, the agglomerating condition is: sintering range is incubated 2 hours at 2000 ℃, and pressure is about 35MPa, and atmosphere is Ar.
Alternative stacked in the step 3 is a multilayer.
The multilayer of alternative stacked is A layer and two B layer crossing stacks.
The multilayer of alternative stacked is a plurality of A layers and a plurality of B layer crossing stack (A+B+B+A+B+B...).
Claims (4)
1. fine and close ultrahigh-temperature multilayer ceramic preparation methods is characterized in that step is following:
Step 1: with ZrB
2, 20～40vol% SiC and less than the B of 10vol%
4Carry out ball milling in C adding 50～60vol% zero(ppm) water and the 1.9～2vol% dispersion agent TMAH; The sticker PVA solution and the 6～7vol% softening agent 1 that add 20～30vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 500～1000 μ m, behind the knifing at air drying and be prepared into A laminin base; The concentration of said PVA solution is 5%; Above-mentioned each percent by volume is for accounting for ZrB
2The percent by volume of powder volume;
Step 2: with the B of SiC and 5vol%
4Carry out ball milling in C adding 50～60vol% zero(ppm) water and the 0.6～0.7vol% dispersion agent TMAH; The sticker PVA solution and the 6～7vol% softening agent 1 that add 20～30vol% again; Ammediol carries out secondary ball milling; In vacuum tightness is to carry out froth in vacuum among the 0.085Mpa to make casting slurry, and the thickness of controlling the base sheet through the height of the embedded sheet glass of curtain coating mould then is 500～1000 μ m, behind the knifing at air drying and be prepared into B laminin base; Above-mentioned each percent by volume is the percent by volume that accounts for SiC powder volume;
Step 3: with A laminin base and the B laminin base alternative stacked after the cutting that requires according to sample, through isostatic cool pressing premolding, pressure is 189MPa, dwell time 60s, one-level release time 30s, secondary release time 8s;
Step 4: place graphite jig to be incubated 1 hour down at 500 ℃ and carry out binder removal, carry out hot pressed sintering then, the agglomerating condition is: sintering range is incubated 2 hours at 1850 ℃～2000 ℃, and pressure is about 35MPa, and atmosphere is Ar.
2. fine and close ultrahigh-temperature multilayer ceramic preparation methods according to claim 1, it is characterized in that: the alternative stacked in the step 3 is a multilayer.
3. fine and close ultrahigh-temperature multilayer ceramic preparation methods according to claim 1 and 2 is characterized in that: the multilayer of alternative stacked is A layer and B layer crossing stack.
4. fine and close ultrahigh-temperature multilayer ceramic preparation methods according to claim 1 and 2 is characterized in that: the multilayer of alternative stacked is a plurality of A layers and a plurality of B layer crossing stack.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058711A (en) * | 2012-12-14 | 2013-04-24 | 西北工业大学 | Method for preparing UHTC (Ultra-High Temperature Ceramic) matrix composite material through modification of UHTC powder basal body |
| CN109534827A (en) * | 2018-12-11 | 2019-03-29 | 莱芜亚赛陶瓷技术有限公司 | A kind of preset interface hot pressing bulletproof ceramic plate and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844925A (en) * | 2010-05-21 | 2010-09-29 | 李艳 | Process for preparing multilayer ZrB2-SiC complex phase ultrahigh temperature ceramic wafer material by tape casting |
| CN101863071A (en) * | 2009-04-15 | 2010-10-20 | 中国科学院上海硅酸盐研究所 | Aqueous tape casting method of superhigh-temperature ceramic |
| CN102225868A (en) * | 2011-04-13 | 2011-10-26 | 中材高新材料股份有限公司 | Preparation of zirconium diboride-silicon carbide ultrahigh-temperature ceramic by slip-casting molding non-pressurized sintering method |
-
2011
- 2011-11-27 CN CN2011103827582A patent/CN102491754A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863071A (en) * | 2009-04-15 | 2010-10-20 | 中国科学院上海硅酸盐研究所 | Aqueous tape casting method of superhigh-temperature ceramic |
| CN101844925A (en) * | 2010-05-21 | 2010-09-29 | 李艳 | Process for preparing multilayer ZrB2-SiC complex phase ultrahigh temperature ceramic wafer material by tape casting |
| CN102225868A (en) * | 2011-04-13 | 2011-10-26 | 中材高新材料股份有限公司 | Preparation of zirconium diboride-silicon carbide ultrahigh-temperature ceramic by slip-casting molding non-pressurized sintering method |
Non-Patent Citations (1)
| Title |
|---|
| 马国佳等: "硼离子注入对SiC-C/SiC复合材料抗氧化性影响", 《复合材料学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058711A (en) * | 2012-12-14 | 2013-04-24 | 西北工业大学 | Method for preparing UHTC (Ultra-High Temperature Ceramic) matrix composite material through modification of UHTC powder basal body |
| CN109534827A (en) * | 2018-12-11 | 2019-03-29 | 莱芜亚赛陶瓷技术有限公司 | A kind of preset interface hot pressing bulletproof ceramic plate and preparation method thereof |
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Application publication date: 20120613 |