CN101920958A - Method for preparing nano zirconium carbide - Google Patents
Method for preparing nano zirconium carbide Download PDFInfo
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- CN101920958A CN101920958A CN2010102470107A CN201010247010A CN101920958A CN 101920958 A CN101920958 A CN 101920958A CN 2010102470107 A CN2010102470107 A CN 2010102470107A CN 201010247010 A CN201010247010 A CN 201010247010A CN 101920958 A CN101920958 A CN 101920958A
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- zirconium carbide
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Abstract
The invention relates to a method for preparing nano zirconium carbide. In the production of the conventional nano zirconium carbide, a catalyst is not added, so the carbonization is nonuniform, the densification degree is low, the sintering property is good, the purity is low and the particle size is nonuniform. In the method, zirconium dioxide and carbon black and an additive are mixed uniformly according to a ratio, the mixture is subjected to carbonization in an oven, and the nano zirconium carbide powder is obtained by screening and ball milling, the carbonization process is implemented by the diffusion of carbon in the zirconium dioxide through the reaction of a carbon-containing gas phase, the zirconium carbide grains are react more quickly through reaction under the high-heat reaction and bonding action of the additive, and the nano zirconium carbide is high in purity, uniform in carbonization, high in densification degree and good in sintering property.
Description
Technical field:
The invention belongs to new metal powder material technical field, be specifically related to a kind of method for formulating of nano-zirconium carbide.
Background technology:
As everyone knows, have the production preparation of traditional nano-zirconium carbide now, in the production preparation process, do not add catalyzer, cause carbonization inhomogeneous, cause closeization degree low, sintering character is poor, and the pure end is low, and granularity is poor, influenced the Application and Development of non-ferrous metal and Rare Metals Materials, the high-end material aspect that has is dependence on import always, has wasted national great amount of manpower and material resources, financial resources, has hindered the development of China's powder metallurgy industry.
Summary of the invention:
The objective of the invention is according to above-mentioned technological deficiency, and provide a kind of method for formulating of nano-zirconium carbide, it has solved the existing technological deficiency that zirconium carbide produces of receiving effectively, the product purity that it is produced is low, carbonization is even, densification degree good, sintering character is good, it has adopted picking of raw material, utilize the manufacture method of microwave carbonization, crystal is well grown up.Compare with the nano-zirconium carbide of usual manner production, can obtain organizing more even, compactness is good, and sintering character is good, and product purity is up to more than 99.9%, epigranular, and its product can reach following technical indicator.
T.C：11.30-11.60％ O：＜0.5％
F.C：＜0.5％ BET(m
2/g)：＞70
SCOTT(g.cm
3)：0.06-0.10
Foreign matter content (being not more than):
Fe：0.020％ Si：0.020％ Na：0.001％ Ca：0.001％
Ti：0.001％ Al：0.001％ Nb：0.001％ N：0.010％
Technical scheme of the present invention be achieved in that the present invention be with zirconium dioxide and carbon black, additive by carrying out the proportioning uniform mixing than row, in microwave oven, carry out carbonization.Through screening, ball milling operation, produce the nano-zirconium carbide powder.Carbonization process mainly is to spread in zirconium dioxide by carbonaceous gas-phase reaction to realize, by the high fever reaction and the cohesive action of additive, impels zirconium carbide crystal grain to react completely rapidly, and combines closely mutually simultaneously.
The carburizing reagent formula:
ZrO
2+3C＝Zrc+2CO
In the carbonization process, therefore zirconium dioxide and charcoal bonded degree direct influence, control the combined carbon content and the compactness extent of nano-zirconium carbide by adjusting parameters such as carbonization temperature, time, boat charge to the combined carbon content of nano-zirconium carbide.
A joins charcoal and mixes:
Raw material: Zirconium dioxide powder (require the purity of zirconium dioxide to be greater than 99.9%, granularity is-400 orders).
B additive and addition.
Zirconium dioxide powder is when joining the charcoal mixing, and adding additive A, two kinds of materials of B (A, B) are respectively sodium-chlor (NaCl) and trioxymethylene (C3H603), and the ratio of its interpolation is respectively 0.3-0.5%, 0.5-0.7%.
C joins the charcoal amount:
The dosage of zirconium dioxide: 70-80%
Sooty dosage: 20-30%
The dosage of additive: 0.8-1.2%
D joins charcoal hybrid technique (carrying out) in the V-type mixing tank
Weight of material: 200-300 (kg/ criticizes);
Mixing time: 150-300 (minute);
E carbonization (in microwave oven, carrying out)
Raw material: the compound that mixes " Zirconium dioxide powder+carbon black+additive ".Visual compound should not have carbon black and additive segregation.
The f carbonization technique
Carry out in industrial microwave oven, concrete processing parameter is:
Boat charge: 1-2 (kg/ boat); Push away boat speed: 30-60 (minute/boat);
Temperature: 800-1200 (℃).
The technological process of production:
Smart titanium dioxide zirconium powder, carbon black, additive joined to be mixed with join charcoal in the device and mix, after enter the microwave carbonization again, after entering 400 mesh sieves again and dividing, enter the analytical study packing after entering the ball mill ball milling, become qualified product, the basic characteristics of nano-zirconium carbide and purposes.
The basic characteristics of nano-zirconium carbide and purposes
The metal ceramic powder that nano-zirconium carbide is a kind of homogeneous microstructure, purity height, epigranular, densification degree is good, sintering character is good, impurity content is low.Selected raw material utilizes the manufacture of microwave carbonization, and crystal is well grown up.Compare with the nano-zirconium carbide that the conventional mode of production is produced, can obtain the more excellent nano-zirconium carbide of quality product, and produce zirconium carbide saves energy 80% than ordinary method.
The nano level metal ceramic powder has excellent performance, and it is applied in a lot of fields.Because its high hardness, the nano-zirconium carbide metal ceramic powder can be used as abrasive material, is used for the processing of various hard metals, corundum or glass; Also can produce wear-resisting, corrosion resistant zirconium carbide crucible and cutter, owing to be nano material, high-end products such as available nano hard alloy and aerospace; Can also be used for the wear-resistant protection film on nuclear fuel industry, electronics, the instrument and the electron emissive film of high brightness in addition.Choose the zirconium carbide coating that different processing condition can obtain different performance, low-density loose zirconium carbide coating thermal stress resistance and insulating property are good.
Description of drawings:
Accompanying drawing is technological process of production figure of the present invention.
Embodiment:
Have only enterprise of several family can produce this series products at present abroad, the production of this series products abroad is directly to produce from zircon by utilizing thermite reaction to generate heat, and grain growth carries out in melt metal menstruum pond.
Our production technique is the top layer of the reactive gas molecular energy rapid permeability reactant that decomposes under lower temperature, has shortened the reaction times, technology with compared a great difference abroad, adopt advanced carbonization technique, with zirconium dioxide (ZrO
2) powder is raw material, allocates required amounts of carbon black into, adds the additive sodium chloride (NaCl) of 0.8-1.2% and trioxymethylene (C3H603) promotor and the catalyzer as carbonization again.Its is shortened time, has reduced production energy consumption, make carburizing reagent fully complete simultaneously, can improve the compactness and the sintering character of product in addition, guarantee the quality of product, make product purity up to more than 99.9%, compactness is good, epigranular.Compare with traditional method, the adding of these two kinds of catalyzer can improve the speed of response of 80% carbonization, can reduce by 20% carbonation reaction temperature, can make the product densification degree improve 50%.
The production unit aspect adopt the microwave reaction producer to replace traditional carbon tube furnace, and the combined process characteristics is transformed to the microwave reaction producer.
Well heater for microwave reaction producer cavity, each pattern all characterizes with a sharp-pointed resonance response on given frequency, have only and make enough overlapping and provide impedance matching preferably at microwave source operating frequency section interior resonance curve when inserting load, could microwave power be coupled in the load successive, load is transmitted bigger power.Because the heating uniformity of this pattern is poor, and very difficult Accurate Analysis, entirely by test design.At these practical situation, by test many times, we propose to adopt transformed single mode resonator, thereby preferably resolve the problem of heating uniformity difference, meet the requirement of production technique.When improving the quality of products, reduce production cost again, saved the energy.And also reduced carbonization temperature, temperature of reaction is controlled at the 800-1000 degree.Produce zirconium carbide save energy 80% than ordinary method.
Defectives such as the external nano-zirconium carbide of producing exists carbonization inhomogeneous, and densification degree is low, and sintering character purity is low, and granularity is inhomogeneous.And the nano-zirconium carbide metal ceramic powder that this technology makes has following characteristics: purity height (＞99.9%), and combined carbon height (＞11.3%), uncombined carbon is low, and (＜0.5%, loose density is 0.08g/cm3; The product crystal formation is a cubic structure, even particle size distribution, and intracrystalline subgrain size is even.Detrimental impurity content is few, compactness degree height; This product has high surface, loose density is low, have high temperature resistant, anti-oxidant, intensity is high, hardness is high, thermal conductivity is good, good toughness, be again a kind of important high-melting-point, high strength and corrosion resistant high-temperature structural material, and have an efficient absorption visible light, the characteristic of reflected infrared and energy storage etc.
Powder metallurgy product quality surveillance inspection center assay:
T.C：11.35％ O：0.48％
F.C：0.4％ BET(m2/g)：78
SCOTT(g/cm
3)：0.08
Foreign matter content (being not more than):
Fe：0.015％ Si：0.015％ Na：0.0005％ Ca：0.0005％
Ti：0.0005％ Al：0.0005％ Nb：0.0005％ N：0.005％
The selection of operational path
This project operational path is different from abroad, but has used for reference the production technique of microwave carbonization and carbonization and titanium carbide, and processing parameter is convenient to control.
The selection of additive
Additive is selected foundation: promote crystal grain to grow complete, raising nano-zirconium carbide compactness, the every index of product is not exerted an influence.Selected two kinds of materials of A, B in view of the above, it is complete that these two kinds of materials can promote that nano-zirconium carbide promotes crystal grain to grow, and can improve its compactness again.
Claims (2)
1. the method for formulating of a nano-zirconium carbide is characterized in that method for formulating is as follows:
It with zirconium dioxide and carbon black, additive by carrying out the proportioning uniform mixing than row, in microwave oven, carry out carbonization, through screening ball milling operation, produce the nano-zirconium carbide powder, carbonization process mainly is to spread in zirconium dioxide by carbonaceous gas-phase reaction to realize, by the high fever reaction and the cohesive action of additive, impel zirconium carbide crystal grain to react completely rapidly, and combine closely mutually simultaneously;
The carburizing reagent formula:
ZrO
2+3C＝ZrC+2CO
In the carbonization process, zirconium dioxide and charcoal bonded degree direct influence are to the combined carbon content of nano-zirconium carbide, and it controls the combined carbon content and the compactness extent of nano-zirconium carbide by adjusting parameters such as carbonization temperature, time, boat charge;
A joins charcoal and mixes:
Raw material: Zirconium dioxide powder (require the purity of zirconium dioxide to be greater than 99.9%, granularity is-400 orders), carbon black (require sooty purity to be greater than 99.9%, granularity is-400 orders);
B additive and addition:
Zirconium dioxide powder is when joining the charcoal mixing, and adding additive A, two kinds of materials of B (A, B) are respectively sodium-chlor (NaCl) and trioxymethylene (C3H603), and the ratio of its interpolation is respectively 0.3-0.5%, 0.50-0.7%;
C joins the charcoal amount:
The dosage of zirconium dioxide: 70-80%
Sooty dosage: 20-30%
The dosage of additive: 0.8-1.2%
D. join charcoal hybrid technique (in the V-type mixing tank, carrying out)
Weight of material: 200-300 (kg/ criticizes)
Mixing time: 150-300 (minute)
E carbonization (in microwave oven, carrying out)
Raw material: the compound that mixes " Zirconium dioxide powder+carbon black+additive ", visual compound should not have carbon black and additive segregation;
The f carbonization technique
Carry out in industrial microwave oven, concrete processing parameter is:
Boat charge: 1-2 (kg/ boat) pushes away boat speed: 30-60 (minute/boat)
Temperature: 800-1200 (℃).
2. the method for formulating of nano-zirconium carbide according to claim 1 is characterized in that the technological process of production is as follows:
Titanium dioxide zirconium powder, carbon black, additive joined to be mixed with join in the device after charcoal mixes, enter the microwave carbonization again, enter 400 screenings again after, enter to enter behind the ball mill ball milling and analyze inspection, be packaged as qualified finished product.
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| CN2010102470107A CN101920958A (en) | 2010-08-06 | 2010-08-06 | Method for preparing nano zirconium carbide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173418A (en) * | 2010-12-31 | 2011-09-07 | 长沙伟徽高科技新材料股份有限公司 | Metallic carbide superfine powder used for preparing superfine crystalline cemented hard alloy and preparation process thereof |
| CN104211063A (en) * | 2014-09-17 | 2014-12-17 | 山东理工大学 | Method for preparing rod-like zirconium carbide powder by solid-phase reaction |
| CN104227010A (en) * | 2013-06-14 | 2014-12-24 | 铜仁学院 | Preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction |
| WO2019095715A1 (en) * | 2017-11-15 | 2019-05-23 | 泰州市艾瑞斯克模具有限公司 | High-temperature sensitive nano-material and preparation method therefor |
| CN112777597A (en) * | 2021-03-23 | 2021-05-11 | 上海简巨医学生物工程有限公司 | Niobium carbide nano material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02271919A (en) * | 1989-04-10 | 1990-11-06 | Central Glass Co Ltd | Production of fine powder of titanium carbide |
| WO1995021946A1 (en) * | 1994-02-15 | 1995-08-17 | The Dow Chemical Company | Method of making metallic carbide powders |
| JP2001328806A (en) * | 2000-05-16 | 2001-11-27 | Allied Material Corp | Vanadium carbide powder and method of producing the same |
| CN1348919A (en) * | 2001-11-29 | 2002-05-15 | 华南理工大学 | Microwave synthesis process for nanometer level titaniuym carbide |
| CN101643210A (en) * | 2009-06-29 | 2010-02-10 | 金堆城钼业股份有限公司 | Method for preparing ultrafine carbide powder |
-
2010
- 2010-08-06 CN CN2010102470107A patent/CN101920958A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02271919A (en) * | 1989-04-10 | 1990-11-06 | Central Glass Co Ltd | Production of fine powder of titanium carbide |
| WO1995021946A1 (en) * | 1994-02-15 | 1995-08-17 | The Dow Chemical Company | Method of making metallic carbide powders |
| JP2001328806A (en) * | 2000-05-16 | 2001-11-27 | Allied Material Corp | Vanadium carbide powder and method of producing the same |
| CN1348919A (en) * | 2001-11-29 | 2002-05-15 | 华南理工大学 | Microwave synthesis process for nanometer level titaniuym carbide |
| CN101643210A (en) * | 2009-06-29 | 2010-02-10 | 金堆城钼业股份有限公司 | Method for preparing ultrafine carbide powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173418A (en) * | 2010-12-31 | 2011-09-07 | 长沙伟徽高科技新材料股份有限公司 | Metallic carbide superfine powder used for preparing superfine crystalline cemented hard alloy and preparation process thereof |
| CN104227010A (en) * | 2013-06-14 | 2014-12-24 | 铜仁学院 | Preparation method for synthetizing zirconium carbide nanometer powder by solid-phase reaction |
| CN104211063A (en) * | 2014-09-17 | 2014-12-17 | 山东理工大学 | Method for preparing rod-like zirconium carbide powder by solid-phase reaction |
| WO2019095715A1 (en) * | 2017-11-15 | 2019-05-23 | 泰州市艾瑞斯克模具有限公司 | High-temperature sensitive nano-material and preparation method therefor |
| CN112777597A (en) * | 2021-03-23 | 2021-05-11 | 上海简巨医学生物工程有限公司 | Niobium carbide nano material and preparation method thereof |
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Application publication date: 20101222 |