CN105084380A - Method for preparing hollow rodlike zirconium boride powder - Google Patents
Method for preparing hollow rodlike zirconium boride powder Download PDFInfo
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Abstract
The invention relates to a method for preparing hollow rodlike zirconium boride powder and belongs to the technical field of powder material preparing. The method includes the steps that 1, saccharose and boric acid are added to acetic acid to be stirred for 30 minutes to 50 minutes at the temperature of 75 DEG C to 85 DEG C, and a solution A is obtained; 2, normal propyl alcohol is dropwise added to the solution A to be stirred for 3 hours to 5 hours at the temperature of 60 DEG C to 70 DEG C, and precursor powder is obtained after drying and grinding are conducted; 3, the precursor powder is kept at the temperature of 600 DEG C to 700 DEG C for 3 hours to 5 hours in a muffle furnace; then the precursor powder is put into a sintering furnace, the temperature of the precursor powder rises to 1180 DEG C to 1220 DEG C at the speed of 5 DEG C/min to 8 DEG C/min, and the precursor powder is kept for 1 hours at the temperature of 1180 DEG C to 1220 DEG C in the argon atmosphere; then the temperature of the precursor powder rises to 1550 DEG C at the speed of 5 DEG C/min to 8 DEG C/min, and the precursor powder is kept at the temperature of 1550 DEG C for 2 hours in the argon atmosphere. The prepared rodlike zirconium boride powder is of a hollow structure and has a larger specific surface area than a common rodlike structure, and the rodlike zirconium boride powder is simple in process, safe to operate and low in cost.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of preparation method of hollow bar-shaped zirconium boride powder.
Background technology
At present, the material can being competent at extreme environment requirement mainly concentrates on high-melting-point boride, carbide as ZrB
2, HfB
2, the superhigh temperature ceramic material of the composition such as ZrC, HfC and TaC.In these superhigh temperature ceramic material systems, zirconium boride 99.5004323A8ure because of its there is high stability, high-melting-point (3240 DEG C), high rigidity (Mohs' hardness is 9), good thermal conductivity (thermal conductivity is 23-25W/ (mK)), (conductance is about 1 × 10 to good electroconductibility
8the advantage such as S/m), obtains and pays close attention to widely and apply in the field such as high temperature ceramic material, ceramic matric composite.
In the preparation process of zirconium boride 99.5004323A8ure, the physical aspect of zirconium boride powder, foreign matter content and specific surface area etc. all can affect the practical application of zirconium boride 99.5004323A8ure, and increasing specific surface area helps lend some impetus to the sintering of zirconium boride powder, current zirconium boride powder is based on ball-type, bar-shaped except random form, and the hollow structure report having more bigger serface is less.
Summary of the invention
The object of this invention is to provide a kind of operational safety, cost is low, synthesizes the preparation method of the zirconium boride powder of hollow club shaped structure.
Technical scheme of the present invention is as follows:
The preparation method of hollow bar-shaped zirconium boride powder of the present invention, is that employing sucrose is carbon source, zirconium-n-propylate is zirconium source, boric acid is boron source, is prepared, specifically comprise the following steps by collosol and gel-carbothermic method:
Step 1, add in acetic acid by sucrose and boric acid, at 75 ~ 85 DEG C, stir 30 ~ 50min, obtain solution A, wherein the mol ratio of sucrose and boric acid is 1:7;
Drip zirconium-n-propylate in step 2, the solution A that obtains in step 1, then at 60 ~ 70 DEG C, stir 3 ~ 5h, obtain solution B, wherein, the mol ratio of boric acid and zirconium-n-propylate is 3:1;
Step 3, solution B step 2 obtained are placed in vacuum drying oven, dry 2 ~ 3h at 110 ~ 120 DEG C of temperature, under 0.01 ~ 0.02MPa pressure, and after cooling, grinding, obtains precursor powder;
The synthesis of step 4, zirconium boride powder: precursor powder step 3 obtained is placed in retort furnace, is incubated 3 ~ 5h, takes out after cooling to room temperature with the furnace at 600 ~ 700 DEG C; Then the powder that upper step process obtains is placed in vacuum carbon pipe sintering oven, with the speed of 5 ~ 10 DEG C/min, temperature from ambient is warming up to 1180 ~ 1220 DEG C, under 1180 ~ 1220 DEG C of temperature, argon gas atmosphere, be incubated 1h; Then be warming up to 1550 DEG C with the temperature rise rate of 5 ~ 8 DEG C/min, under 1550 DEG C of temperature, argon gas atmosphere, be incubated 2h, naturally cool to room temperature with stove, namely obtain hollow bar-shaped zirconium boride powder of the present invention.
Beneficial effect of the present invention is:
The bar-shaped zirconium boride powder that the present invention prepares is hollow structure, has the specific surface area larger than common club shaped structure; Sintering temperature is low, and sintering character is good; Preparation technology's simple and stable, operational safety, cost is low, and powder oxygen level is low.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the zirconium boride powder that the embodiment of the present invention 1 prepares;
Fig. 2 is the SEM figure of the zirconium boride powder that the embodiment of the present invention 1 prepares.
Embodiment
Below in conjunction with drawings and Examples in detail technical scheme of the present invention is described in detail.
Embodiment 1
A preparation method for hollow bar-shaped zirconium boride powder, specifically comprises the following steps:
Step 1,2.5g sucrose, 2.97g boric acid are added in 36mL acetic acid, then on magnetic stirring apparatus, at the uniform velocity stir 30min at 80 DEG C, obtain solution A;
Step 2,5.30g zirconium-n-propylate at the uniform velocity to be instilled in solution A that step 1 obtains, then on magnetic stirring apparatus, at the uniform velocity stir 3.5h at 65 DEG C, obtain solution B;
Step 3, solution B step 2 obtained are placed in vacuum drying oven, dry 2h at 110 DEG C of temperature, under 0.01MPa pressure, and after cooling, grinding, obtains precursor powder;
The synthesis of step 4, zirconium boride powder: precursor powder step 3 obtained is placed in retort furnace, is incubated 3h at 600 DEG C, takes out after cooling to room temperature with the furnace; Then the powder of taking-up is placed in vacuum carbon pipe sintering oven, with the speed of 10 DEG C/min, temperature from ambient is warming up to 1200 DEG C, under 1200 DEG C of temperature, argon gas atmosphere, be incubated 1h; Then be warming up to 1550 DEG C with the temperature rise rate of 5 DEG C/min by 1200 DEG C, under 1550 DEG C of temperature, argon gas atmosphere, be incubated 2h, naturally cool to room temperature with stove, namely obtain hollow bar-shaped zirconium boride powder of the present invention.
Fig. 1 is the XRD figure spectrum of the zirconium boride powder that the embodiment of the present invention 1 prepares; As shown in Figure 1, embodiment 1 has successfully prepared zirconium boride powder.Fig. 2 is the SEM figure of the zirconium boride powder that the embodiment of the present invention 1 prepares; As shown in Figure 2, the zirconium boride powder that embodiment 1 obtains is hollow club shaped structure.
Embodiment 2
A preparation method for hollow bar-shaped zirconium boride powder, specifically comprises the following steps:
Step 1,3.00g sucrose, 3.56g boric acid are added in 43mL acetic acid, then on magnetic stirring apparatus, at the uniform velocity stir 40min at 75 DEG C, obtain solution A;
Step 2,6.36g zirconium-n-propylate at the uniform velocity to be instilled in solution A that step 1 obtains, then on magnetic stirring apparatus, at the uniform velocity stir 4h at 60 DEG C, obtain solution B;
Step 3, solution B step 2 obtained are placed in vacuum drying oven, dry 2.5h at 120 DEG C of temperature, under 0.02MPa pressure, and after cooling, grinding, obtains precursor powder;
The synthesis of step 4, zirconium boride powder: precursor powder step 3 obtained is placed in retort furnace, is incubated 4h at 650 DEG C, takes out after cooling to room temperature with the furnace; Then the powder of taking-up is placed in vacuum carbon pipe sintering oven, with the speed of 10 DEG C/min, temperature from ambient is warming up to 1180 DEG C, under 1180 DEG C of temperature, argon gas atmosphere, be incubated 1h; Then be warming up to 1550 DEG C with the temperature rise rate of 5 DEG C/min by 1180 DEG C, under 1550 DEG C of temperature, argon gas atmosphere, be incubated 2h, naturally cool to room temperature with stove, namely obtain hollow bar-shaped zirconium boride powder of the present invention.
Embodiment 3
Step 1,3.50g sucrose, 4.46g boric acid are added in 55mL acetic acid, then on magnetic stirring apparatus, at the uniform velocity stir 50min at 85 DEG C, obtain solution A;
Step 2,7.95g zirconium-n-propylate at the uniform velocity to be instilled in solution A that step 1 obtains, then on magnetic stirring apparatus, at the uniform velocity stir 4.5h at 70 DEG C, obtain solution B;
Step 3, solution B step 2 obtained are placed in vacuum drying oven, dry 3h at 110 DEG C of temperature, under 0.02MPa pressure, and after cooling, grinding, obtains precursor powder;
The synthesis of step 4, zirconium boride powder: precursor powder step 3 obtained is placed in retort furnace, is incubated 5h at 700 DEG C, takes out after cooling to room temperature with the furnace; Then the powder of taking-up is placed in vacuum carbon pipe sintering oven, with the speed of 10 DEG C/min, temperature from ambient is warming up to 1220 DEG C, under 1220 DEG C of temperature, argon gas atmosphere, be incubated 1h; Then be warming up to 1550 DEG C with the temperature rise rate of 5 DEG C/min by 1220 DEG C, under 1550 DEG C of temperature, argon gas atmosphere, be incubated 2h, naturally cool to room temperature with stove, namely obtain hollow bar-shaped zirconium boride powder of the present invention.
Claims (1)
1. a preparation method for hollow bar-shaped zirconium boride powder, comprises the following steps:
Step 1, add in acetic acid by sucrose and boric acid, at 75 ~ 85 DEG C, stir 30 ~ 50min, obtain solution A, wherein the mol ratio of sucrose and boric acid is 1:7;
Drip zirconium-n-propylate in step 2, the solution A that obtains in step 1, then at 60 ~ 70 DEG C, stir 3 ~ 5h, obtain solution B, wherein, the mol ratio of boric acid and zirconium-n-propylate is 3:1;
Step 3, solution B step 2 obtained are placed in vacuum drying oven, dry 2 ~ 3h at 110 ~ 120 DEG C of temperature, under 0.01 ~ 0.02MPa pressure, and after cooling, grinding, obtains precursor powder;
The synthesis of step 4, zirconium boride powder: precursor powder step 3 obtained is placed in retort furnace, is incubated 3 ~ 5h, takes out after cooling to room temperature with the furnace at 600 ~ 700 DEG C; Then the powder that upper step process obtains is placed in vacuum carbon pipe sintering oven, with the speed of 5 ~ 10 DEG C/min, temperature from ambient is warming up to 1180 ~ 1220 DEG C, under 1180 ~ 1220 DEG C of temperature, argon gas atmosphere, be incubated 1h; Then be warming up to 1550 DEG C with the temperature rise rate of 5 ~ 8 DEG C/min, under 1550 DEG C of temperature, argon gas atmosphere, be incubated 2h, naturally cool to room temperature with stove, namely obtain hollow bar-shaped zirconium boride powder of the present invention.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113860878A (en) * | 2021-10-15 | 2021-12-31 | 山东鹏程陶瓷新材料科技有限公司 | Process for preparing rod-like zirconium boride powder at low temperature |
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| CN103588216A (en) * | 2013-10-23 | 2014-02-19 | 航天材料及工艺研究所 | Method for preparing zirconium boride powder at low temperature according to boron/carbon thermal reduction method |
| 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 |
| CN104129995A (en) * | 2014-07-28 | 2014-11-05 | 北京航空航天大学 | Method for synthesis of ZrB2-SiC composite-phase powder through boron thermal reduction and carbon thermal reduction collaborative regulation and control |
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2015
- 2015-08-06 CN CN201510476739.4A patent/CN105084380B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103588216A (en) * | 2013-10-23 | 2014-02-19 | 航天材料及工艺研究所 | Method for preparing zirconium boride powder at low temperature according to boron/carbon thermal reduction method |
| 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 |
| CN104129995A (en) * | 2014-07-28 | 2014-11-05 | 北京航空航天大学 | Method for synthesis of ZrB2-SiC composite-phase powder through boron thermal reduction and carbon thermal reduction collaborative regulation and control |
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| 李锐星 等: ""碳热还原协同溶胶-凝胶法合成棒状纳米ZrB2粉末"", 《中国材料进展》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113860878A (en) * | 2021-10-15 | 2021-12-31 | 山东鹏程陶瓷新材料科技有限公司 | Process for preparing rod-like zirconium boride powder at low temperature |
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