CN105197953A - Synthetic process of rod zirconium boride powder - Google Patents
Synthetic process of rod zirconium boride powder Download PDFInfo
- Publication number
- CN105197953A CN105197953A CN201510628981.9A CN201510628981A CN105197953A CN 105197953 A CN105197953 A CN 105197953A CN 201510628981 A CN201510628981 A CN 201510628981A CN 105197953 A CN105197953 A CN 105197953A
- Authority
- CN
- China
- Prior art keywords
- powder
- zirconium boride
- carbon dust
- argon atmosphere
- bar
- 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
Links
Abstract
The invention provides a synthetic process of rod zirconium boride powder and belongs to the technical field of powdery materials. The synthetic process is characterized by including 1, preparing carbon powder: curing thermosetting phenol resin at 80-120 DEG C, calcining the resin at 200-1500 DEG C in an argon atmosphere at a temperature rise rate of 8-12 DEG C/min, and holding the temperature for 10-30 min to generate carbon powder through splitting; 2, mixing raw materials: crushing the carbon powder, and mixing zirconium tetrachloride, boric acid and the carbon powder according to a molar ratio of 1:2:5; 3, performing sintering: sintering mixed powder at 1650-1750 DEG C in the argon atmosphere, and holding the temperature for 0.5-2 h t to obtain the rod zirconium boride powder. The synthetic process has the advantages that sintering temperature is low, the process is simple, operating is safe, the cost is low, the process is easy to popularize, and the prepared rod zirconium boride powder has good dispersity and a length-diameter ratio increased by 4 times.
Description
Technical field
The invention provides a kind of synthesis technique of bar-shaped zirconium boride powder, belong to technical field of powdered material preparation.
Background technology
Zirconium diboride superhigh temperature ceramics has high-melting-point (3245 DEG C), (Mohs' hardness is 9 to high rigidity, microhardness is 22.1GPa), the premium properties such as high heat conductance (thermal conductivity is 23 ~ 25W/ (mK)), it is a kind of high-temperature structural material of excellent performance, be expected to for various key positions such as aircraft nose cone, nose of wing, numbers of hot-side engine, but due to the fragility that stupalith is intrinsic, it is compared with metallic substance, strength decentralization is large, reliability is low, limits pottery as high reliability part design and use.Therefore, in order to ensure reliability in use procedure and security, ZrB must be improved
2the brittleness problems of pottery, thus improve its thermal shock resistance.
Research shows that the performance of pottery is relevant with the pattern of powder used, as replaced particulate state powder that the fracture toughness property of stupalith can be made to significantly improve by fibrous powder in the preparation of composite ceramics; Using platy shaped particle to substitute spheroidal particle can make the thermal-shock resistance of stupalith increase.Along with the continuous expansion that zirconium boride 99.5004323A8ure is applied in high-tech sector, the zirconium boride powder preparing different-shape has become the another focus of zirconium boride ultrahigh-temperature ceramic investigation of materials.Bar-shaped zirconium boride powder is expected to the fracture toughness property and the thermal-shock resistance that improve zirconium boride 99.5004323A8ure based ultra-high temperature pottery, and make it as high-temperature structural material, during application, safety and reliability is improved.Document " Synthesisofhexagonal-prism-likeZrB
2byasol – gelroute.PowderTechnology, 2014:256,522 – 528 ", with zirconium-n-propylate, glucose, boric acid for raw material, adopt sol-gel method to prepare bar-shaped zirconium boride powder; bar-shaped zirconium boride 99.5004323A8ure diameter is about 0.8 μm; length is about 5 μm, shortcoming is that collosol and gel generates control difficulty, and gel needs suction filtration, composition proportion to be difficult to accurately control; poor repeatability, finished product low conversion rate.
Patent CN103922360A " technique of the bar-shaped zirconium boride powder of low-temperature growth ", with bar-shaped zirconium tetrachloride powder for raw material, be heated to 900 ~ 1100 DEG C of insulation 0.2 ~ 1h, obtain bar-shaped Zirconium powder, then be 1:(2 ~ 2.2 in molar ratio by bar-shaped zirconium white, boric acid, carbon dust): 5 mixing, sinter under an argon atmosphere, sintering temperature is 1500 ~ 1700 DEG C, obtain bar-shaped zirconium boride powder, prepare bar-shaped zirconium boride powder, length-to-diameter ratio is greater than 2 times.Shortcoming first obtains bar-shaped Zirconium powder with zirconium tetrachloride powder calcination, and then mix with boric acid, carbon dust and generate bar-shaped zirconium boride 99.5004323A8ure, reduces sintering reaction powder active; During bar-shaped zirconium white mixing, morphology microstructure is easily destroyed.
Summary of the invention
The object of this invention is to provide a kind of sintering temperature low, technique is simple, operational safety, and cost is low, is easy to the synthesis technique of the bar-shaped zirconium boride powder of industrialization, and its technical scheme is:
1) prepare carbon dust: take heat-reactive phenolic resin as raw material, first solidify at 80 ~ 120 DEG C, then under an argon atmosphere, 1200 ~ 1500 DEG C of calcinings, heat-up rate is 8 ~ 12 DEG C/min, insulation 10 ~ 30min, and cracking generates carbon dust; 2) raw material mixing: first that carbon dust is broken, then by 1: 2: 5 mixing in molar ratio of zirconium tetrachloride, boric acid and carbon dust; 3) sinter: by the powder mixed, sinter under an argon atmosphere, sintering temperature is 1650 ~ 1750 DEG C, and soaking time is 0.5 ~ 2h, obtains bar-shaped zirconium boride powder.
compared with prior art, tool has the following advantages in the present invention:
1, the present invention prepares bar-shaped zirconium boride powder, and length-to-diameter ratio is greater than 4 times;
2, in sintering process, hydrogenchloride and CO (carbon monoxide converter) gas are released in reaction, further increase the dispersiveness of powder;
3, adopt zirconium tetrachloride, boric acid and carbon dust directly to mix, contrast original technology and first generate zirconium white, then mix with boric acid and carbon dust, simplify preparation technology;
4, the present invention prepares the technique of bar-shaped zirconium boride powder, and technique is simple, and operational safety, cost is low, is easy to industrialization.
Accompanying drawing explanation
Fig. 1 is the XRD spectrum that the present invention prepares powder;
Fig. 2 is the SEM photo that the present invention prepares powder.
Embodiment
Embodiment 1
1) prepare carbon dust: take heat-reactive phenolic resin as raw material, first solidify at 80 DEG C, then under an argon atmosphere, 1200 DEG C of calcinings, heat-up rate is 8 DEG C/min, insulation 10min, and cracking generates carbon dust;
2) raw material mixing: first that carbon dust is broken, then by 1: 2: 5 mixing in molar ratio of zirconium tetrachloride, boric acid and carbon dust;
3) sinter: by the powder mixed, sinter under an argon atmosphere, sintering temperature is 1650 DEG C, and soaking time is 2h, obtains bar-shaped zirconium boride powder.
Tested by XRD, visible powder is zirconium diboride (see figure 1); Tested by SEM, visible Zirconium powder is bar-shaped, and diameter is about 2 μm, and length is about 8 μm (see figure 2)s.
Embodiment 2
1) prepare carbon dust: take heat-reactive phenolic resin as raw material, first solidify at 120 DEG C, then under an argon atmosphere, 1500 DEG C of calcinings, heat-up rate is 12 DEG C/min, insulation 30min, and cracking generates carbon dust;
2) raw material mixing: first that carbon dust is broken, then by 1: 2: 5 mixing in molar ratio of zirconium tetrachloride, boric acid and carbon dust;
3) sinter: by the powder mixed, sinter under an argon atmosphere, sintering temperature is 1750 DEG C, and soaking time is 0.5h, obtains bar-shaped zirconium boride powder.
Embodiment 3
1) prepare carbon dust: take heat-reactive phenolic resin as raw material, first solidify at 100 DEG C, then under an argon atmosphere, 1400 DEG C of calcinings, heat-up rate is 10 DEG C/min, insulation 20min, and cracking generates carbon dust;
2) raw material mixing: first that carbon dust is broken, then by 1: 2: 5 mixing in molar ratio of zirconium tetrachloride, boric acid and carbon dust;
3) sinter: by the powder mixed, sinter under an argon atmosphere, sintering temperature is 1700 DEG C, and soaking time is 1h, obtains bar-shaped zirconium boride powder.
Embodiment 4
1) prepare carbon dust: take heat-reactive phenolic resin as raw material, first solidify at 110 DEG C, then under an argon atmosphere, 1300 DEG C of calcinings, heat-up rate is 9 DEG C/min, insulation 30min, and cracking generates carbon dust;
2) raw material mixing: first that carbon dust is broken, then by 1: 2: 5 mixing in molar ratio of zirconium tetrachloride, boric acid and carbon dust;
3) sinter: by the powder mixed, sinter under an argon atmosphere, sintering temperature is 1750 DEG C, and soaking time is 0.5h, obtains bar-shaped zirconium boride powder.
Claims (1)
1. the synthesis technique of a bar-shaped zirconium boride powder, it is characterized in that: 1) prepare carbon dust: take heat-reactive phenolic resin as raw material, first solidify at 80 ~ 120 DEG C, then under an argon atmosphere, 1200 ~ 1500 DEG C of calcinings, heat-up rate is 8 ~ 12 DEG C/min, insulation 10 ~ 30min, and cracking generates carbon dust; 2) raw material mixing: first that carbon dust is broken, then by 1: 2: 5 mixing in molar ratio of zirconium tetrachloride, boric acid and carbon dust; 3) sinter: by the powder mixed, sinter under an argon atmosphere, sintering temperature is 1650 ~ 1750 DEG C, and soaking time is 0.5 ~ 2h, obtains bar-shaped zirconium boride powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510628981.9A CN105197953A (en) | 2015-09-29 | 2015-09-29 | Synthetic process of rod zirconium boride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510628981.9A CN105197953A (en) | 2015-09-29 | 2015-09-29 | Synthetic process of rod zirconium boride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105197953A true CN105197953A (en) | 2015-12-30 |
Family
ID=54945989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510628981.9A Pending CN105197953A (en) | 2015-09-29 | 2015-09-29 | Synthetic process of rod zirconium boride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105197953A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249688A (en) * | 2011-05-25 | 2011-11-23 | 山东理工大学 | Method for preparing zirconium boride powder |
| CN103922360A (en) * | 2014-03-26 | 2014-07-16 | 山东理工大学 | Process of preparing rod-like zirconium boride powder at low temperature |
-
2015
- 2015-09-29 CN CN201510628981.9A patent/CN105197953A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249688A (en) * | 2011-05-25 | 2011-11-23 | 山东理工大学 | Method for preparing zirconium boride powder |
| CN103922360A (en) * | 2014-03-26 | 2014-07-16 | 山东理工大学 | Process of preparing rod-like zirconium boride powder at low temperature |
Non-Patent Citations (2)
| Title |
|---|
| J. K. SONBER ET AL.: "Synthesis and consolidation of zirconium diboride: review", 《ADVANCES IN APPLIED CERAMICS》 * |
| MATTHEW THOMPSON ET AL.: "Effect of Starting Particle Size and Oxygen Content on Densification of ZrB2", 《J. AM. CERAM. SOC.》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103408315B (en) | Three-dimensional mesophase pitch-based carbon/carbon composite material with high heat conductivity and preparation technology thereof | |
| CN103922778B (en) | Three-dimensional alumina fiber fabric reinforced oxide ceramic and preparation method thereof | |
| CN103922360B (en) | The technique of the bar-shaped zirconium boride powder of low temperature preparation | |
| CN104150940B (en) | Silicon nitride and silicon carbide complex phase porous ceramics and preparation method thereof | |
| Li et al. | Fabrication and comparison of 3D Cf/ZrC–SiC composites using ZrC particles/polycarbosilane and ZrC precursor/polycarbosilane | |
| CN109704800A (en) | One kind being based on the molding short carbon fiber toughened ceramic composite forming method of direct write | |
| CN106882974B (en) | Preparation method of C/HfC-SiC composite material with high HfC content | |
| CN105152670B (en) | A kind of preparation method of SiC nanowire enhancing SiBCN ceramics | |
| CN105110809A (en) | Preparation method for graphene-modified high thermal conductivity three-dimensional carbon/carbon composite material | |
| CN105237034A (en) | Method for preparing porous silicon carbide ceramic based on template | |
| CN109265187A (en) | A kind of Cf/HfC-TaC-C composite material and preparation method | |
| CN106915961A (en) | A kind of Graphene zirconium oxide composite material and preparation method thereof | |
| CN102976760A (en) | RE2O3-added ZrB2-SiC composite ceramic material and preparation method thereof | |
| CN112500167A (en) | Preparation method of densified titanium carbide composite ceramic | |
| CN103288454A (en) | Method for preparing ZrC-SiC composite ceramic material | |
| WO2011011603A2 (en) | Glass encapsulated hot isostatic pressed silicon carbide | |
| CN104261822B (en) | A kind of zirconia composite ceramics and preparation method thereof | |
| CN103803950B (en) | Boron nitride nanotube reinforced ceramic-based composite material and preparation method thereof | |
| CN104844214B (en) | Densified high-strength zirconium carbide ceramic material, densified high-strength hafnium carbide ceramic material, and low temperature preparation methods of densified high-strength zirconium carbide ceramic material and densified high-strength hafnium carbide ceramic material | |
| CN105197953A (en) | Synthetic process of rod zirconium boride powder | |
| CN105197954A (en) | Synthetic method of rod zirconium boride powder | |
| CN104328496A (en) | Preparation method of aluminum borate whisker | |
| CN103253941B (en) | High-heat conductance ZrB2 high-temperature ceramics and preparation method thereof | |
| CN105272267A (en) | Preparation technology of intragranular ZrB2 based UHTCs (ultra-high temperature ceramics) | |
| CN105152180A (en) | Preparation process of hollow rod-like zirconium boride powder |
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: 20151230 |
|
| RJ01 | Rejection of invention patent application after publication |