CN109279605A - A kind of hafnium carbide preparation method - Google Patents
A kind of hafnium carbide preparation method Download PDFInfo
- Publication number
- CN109279605A CN109279605A CN201811433925.XA CN201811433925A CN109279605A CN 109279605 A CN109279605 A CN 109279605A CN 201811433925 A CN201811433925 A CN 201811433925A CN 109279605 A CN109279605 A CN 109279605A
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- China
- Prior art keywords
- glucide
- hafnium oxide
- hafnium
- hafnium carbide
- present
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention provides a kind of preparation method of hafnium carbide powder, including glue, stirring, drying, three-stage sintering, broken process.Firstly, glucide is dissolved in water, sticky mass is formed, nanoscale or micron-sized hafnium oxide powder is then added, is thoroughly mixed uniformly.Three-stage sintering is then carried out in vacuum carbon tube furnace.The sintered substance of gained obtains hafnium carbide product after broken.Present invention process is simple, and product purity is high, and operation is few, at low cost, is conducive to large-scale promotion.
Description
Technical field
The invention belongs to chemosynthesis technical fields, and in particular to a kind of hafnium carbide preparation method.
Background technique
Hafnium carbide has the good characteristics such as high-melting-point (3980 DEG C), high rigidity, the good, good conductivity of thermal stability, in micro- electricity
There is good application prospect in the fields such as son, nuclear energy, aerospace.
Currently, the synthetic method for the hafnium carbide reported both at home and abroad mainly has: 1. direct carbothermic methods, using graphite and oxygen
After changing hafnium solid phase mixing, hafnium carbide product is obtained in 1900 DEG C of high temperature sinterings, this method solid phase mixing uniformity is poor, and product is pure
Degree influences higher.2. using HfOCl2With the raw materials such as hydrochloric acid, n-butanol, the different hafnium carbide of granule-morphology is prepared at 1500 DEG C
Powder, granule has serious reunion situation.3. chemical vapour deposition technique is used, with HfCl4With suitable CH4And H2For raw material, system
Standby hafnium carbide out, the method time length, low yield, method difficulty are big.
The mixing uniformity existing for the current production technology is poor, low output, purity difference aiming at the problem that, the present invention proposes to utilize
Sintering technology after liquid carbon precursor and hafnium oxide powder mixing, obtains high-purity hafnium carbide powder, and realize engineering.
Summary of the invention
Present invention seek to address that the problems such as reaction uniformity existing in the prior art is poor, low output, high impurity content, mentions
It is uniformly mixed out using excessive thick glucide and hafnium oxide, so as to guarantee hafnium oxide and carbon in high temperature sintering
Reaction obtains high-purity hafnium carbide product completely.
The technical scheme is that a kind of hafnium carbide preparation method, comprising the following steps:
Step 1: glucide being dissolved in water stirring, temperature is controlled at 25-80 DEG C, forms sticky mass.By oxygen
Change hafnium powder, which is added in sticky mass, to be stirred.
Step 2: the substance after stirring being transferred in vacuum carbon tube furnace, three-stage sintering is carried out.
Step 3: after self-heating cooling, taking out powder, can be obtained product after broken.
Further, the hafnium carbide powder preparation method, it is characterised in that carbohydrate is formed into viscous liquid, then plus
Enter available uniformly mixed pureed material after hafnium oxide powder.
Further, the three-stage sintering are as follows: first 150-300 DEG C is to slowly warm up under an inert atmosphere, by carbohydrate object
Matter carbonization 2-5h；It is continuously heating to 1500-2000 DEG C of progress high temperature sintering 6-12h；Finally it is cooled to 500-700 DEG C of air atmosphere
Lower calcination 6-12h.
Further, the hafnium carbide powder preparation method, it is characterised in that carbon and oxygen in the glucide
The molar ratio for changing hafnium is higher than 1, optimal value 1.5-3.
Further, the hafnium carbide powder preparation method, it is characterised in that the glucide can be grape
The combination of one or more of sugar, sucrose, fructose.
Further, the inert atmosphere is mainly argon gas.
Beneficial effects of the present invention have the advantage that compared with prior art
The present invention forms thick liquid using carbohydrate, is conducive to uniformly wrap up in hafnium oxide surface, so that entire anti-
Should uniformly, hafnium oxide content is low in product.
For the present invention using three-stage sintering technology in same equipment, process is simple, easy to operate, is conducive to engineering amplification.
Detailed description of the invention
Fig. 1 is hafnium carbide preparation method implementing process process of the present invention.
Fig. 2 is hafnium carbide powder XRD spectrum prepared by the embodiment of the present invention 1.
Fig. 3 is hafnium carbide powder XRD spectrum prepared by the embodiment of the present invention 2.
Table 1 is hafnium carbide powder purity test result prepared by the embodiment of the present invention 1 and 2.
Specific embodiment:
Present invention will be further explained below with reference to the attached drawings and examples, it should be noted that for these embodiments
Description, only intercepted certain required material or some way, be used to help understand the content of present invention, not constitute
Limitation of the invention.
Embodiment 1
It takes 1000kg glucose to be put into 500ml water to stir, stirring is to thick, without being completely dissolved.Then
It is added 50g hafnium oxide powder (100nm-3 μm of partial size).Material is maintained as pureed after the completion of stirring.The pug that will be stirred
Be placed in vacuum carbon tube furnace, be passed through argon gas, be slowly raised to 200 DEG C using the rate of 1 DEG C/min, keep the temperature 5h, continue thereafter with
10 DEG C/min heating rate is raised to 1500 DEG C of sintering 6h, is then cooled to 500 DEG C with 10 DEG C/min rate, is at this time changed to atmosphere
Air with furnace is down to room temperature after keeping the temperature 6h.Then the material being sintered is taken out, can be obtained using broken crusher machine post package
Product carries out XRD object and mutually tests, and surveys free state carbon content using weight-loss method and tests oxygen content using infrared absorption method.
Embodiment 2
It takes 1000kg sucrose to be put into 500ml water to stir, stirring is to thick, without being completely dissolved.Then add
Enter 100g hafnium oxide powder (100nm-3 μm of partial size).Material is maintained as pureed after the completion of stirring.The pug being stirred is set
In vacuum carbon tube furnace, it is passed through argon gas, 200 DEG C is slowly raised to using the rate of 1 DEG C/min, keeps the temperature 5h, continue thereafter with 10
DEG C/min heating rate is raised to 1800 DEG C of sintering 12h, 600 DEG C then are cooled to 10 DEG C/min rate, is at this time changed to atmosphere
Air with furnace is down to room temperature after keeping the temperature 12h.Then the material being sintered is taken out, can be obtained using broken crusher machine post package
Product is obtained, XRD object is carried out and mutually tests, free state carbon content is surveyed using weight-loss method and oxygen content is tested using infrared absorption method.
Subordinate list 1
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of hafnium carbide preparation method, it is characterised in that: the following steps are included:
1) glucide is dissolved in water stirring, forms sticky mass, hafnium oxide powder is added in sticky mass
It stirs evenly；
2) step 1) gains are transferred in vacuum carbon tube furnace, carry out three-stage sintering；
3) by after step 2) gains Temperature fall, being crushed can be obtained product.
2. method according to claim 1, which is characterized in that be dissolved in 25-80 DEG C of progress described in step 1).
3. method according to claim 1, which is characterized in that carbon and hafnium oxide in glucide described in step 1) rub
You are than being higher than 1.
4. method according to claim 1, which is characterized in that carbon and hafnium oxide in glucide described in step 1) rub
You are than being 1.5-3.
5. method according to claim 1, which is characterized in that glucide described in step 1) is glucose, sucrose, fructose
One or more of combination.
6. method according to claim 1, which is characterized in that gains are uniformly mixed pureed material in step 1).
7. method according to claim 1, which is characterized in that the partial size of hafnium oxide powder described in step 1) is 100nm-3 μ
m。
8. method according to claim 1, which is characterized in that vacuum drying oven described in step 2) is Vacuum graphite oven.
9. method according to claim 1, which is characterized in that three-stage sintering described in step 2) are as follows: first under an inert atmosphere
It is to slowly warm up to 150-300 DEG C, glucide is carbonized 2-5h；It is continuously heating to 1500-2000 DEG C of progress high temperature sintering 6-
12h；Finally it is cooled to calcination 6-12h under 500-700 DEG C of air atmosphere.
10. method according to claim 9, which is characterized in that inert atmosphere described in step 2) is mainly argon gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811433925.XA CN109279605A (en) | 2018-11-28 | 2018-11-28 | A kind of hafnium carbide preparation method |
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| CN201811433925.XA CN109279605A (en) | 2018-11-28 | 2018-11-28 | A kind of hafnium carbide preparation method |
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| CN109279605A true CN109279605A (en) | 2019-01-29 |
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| CN201811433925.XA Pending CN109279605A (en) | 2018-11-28 | 2018-11-28 | A kind of hafnium carbide preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113924270A (en) * | 2019-04-15 | 2022-01-11 | 中部电力株式会社 | Hafnium carbide powder for plasma electrode, method for producing same, hafnium carbide sintered body, and plasma electrode |
| CN115259163A (en) * | 2022-07-19 | 2022-11-01 | 宁波合盛新材料有限公司 | Synthesis method of cerium silicide |
| CN116854092A (en) * | 2023-07-28 | 2023-10-10 | 北京华威锐科化工有限公司 | Hafnium carbide precursor production system and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253669A (en) * | 2013-05-17 | 2013-08-21 | 航天材料及工艺研究所 | Method for preparing HfC powder at low temperature by carbothermic method |
| KR101633448B1 (en) * | 2014-12-18 | 2016-06-24 | 한국기계연구원 | A HfC Powder and A Manufacturing method of the same |
| CN105732043A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing hafnium carbide ceramic powder body by using fused salt under assistance of carbon thermal reduction |
-
2018
- 2018-11-28 CN CN201811433925.XA patent/CN109279605A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253669A (en) * | 2013-05-17 | 2013-08-21 | 航天材料及工艺研究所 | Method for preparing HfC powder at low temperature by carbothermic method |
| KR101633448B1 (en) * | 2014-12-18 | 2016-06-24 | 한국기계연구원 | A HfC Powder and A Manufacturing method of the same |
| CN105732043A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing hafnium carbide ceramic powder body by using fused salt under assistance of carbon thermal reduction |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113924270A (en) * | 2019-04-15 | 2022-01-11 | 中部电力株式会社 | Hafnium carbide powder for plasma electrode, method for producing same, hafnium carbide sintered body, and plasma electrode |
| CN115259163A (en) * | 2022-07-19 | 2022-11-01 | 宁波合盛新材料有限公司 | Synthesis method of cerium silicide |
| CN115259163B (en) * | 2022-07-19 | 2023-10-10 | 宁波合盛新材料有限公司 | Synthesis method of cerium silicide |
| CN116854092A (en) * | 2023-07-28 | 2023-10-10 | 北京华威锐科化工有限公司 | Hafnium carbide precursor production system and preparation method |
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