CN107311697A - One kind production VN alloy saggar protective layer and preparation method thereof - Google Patents
One kind production VN alloy saggar protective layer and preparation method thereof Download PDFInfo
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- CN107311697A CN107311697A CN201710643782.4A CN201710643782A CN107311697A CN 107311697 A CN107311697 A CN 107311697A CN 201710643782 A CN201710643782 A CN 201710643782A CN 107311697 A CN107311697 A CN 107311697A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/515—Other specific metals
- C04B41/5155—Aluminium
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Abstract
One kind production VN alloy saggar protective layer and preparation method thereof; the protective layer is uniformly applied to the inside and outside layer surface of vanadium-nitrogen alloy sintering saggar; mixed and be made by solid powder and organic solvent, the component of solid powder includes 70 ~ 85wt% of mullite, 10 ~ 22wt% of carborundum, 2.0 ~ 5.0wt% of Sialon ceramics powder, 0.5 ~ 2.0wt% of metallic aluminium powder, 0.5 ~ 2.0wt% of metallic silicon power by mass percentage；The component of organic solvent includes liquid phenolic resin and absolute alcohol, and the ratio of liquid phenolic resin and absolute alcohol by weight percentage is：70~90wt%：10~30wt%；The ratio of solid powder and organic solvent agent by weight percentage is 100wt%：30~50wt%.The production VN alloy being made averagely improves 28.6% with body service life, and cost averagely have dropped 18.82%.
Description
Technical field
The present invention relates to vanadium-nitrogen alloy sintering device field, more particularly to production VN alloy sintering saggar.
Background technology
VN alloy can improve intensity, toughness, ductility and the thermal fatigue resistance of steel as a kind of new steel additive agent
Deng comprehensive mechanical performance, and make steel that there is good solderability.In the case where reaching same intensity, addition VN alloy relatively adds vanadium can
Save vanadium 30%~40%.As state compulsion requires that building bar intensity must reach more than HRB400, VN alloy market
There is rapid growth in demand.
It is to be made using high pressure marble forming machine after VN alloy green-ball to produce VN alloy, and VN alloy green-ball is put into sintering
In saggar, subsequent body is sent in tunnel cave or pushed bat kiln and is sintered.Sintering body is made up of graphite at present, is vanadium nitrogen
One of cost maximum is accounted for during alloy production in easily-consumed products, its reason is analyzed, mainly has：【1】Graphite product rupture strength
Bottom, it is easy to which cracking disintegrates under external force in process of production.【2】Load VN alloy green-ball and removal in body solid
During the VN alloy finished ball melted, material produces larger impact and friction with body, causes sintering body loss.【3】Vanadium nitrogen
Cold and hot temperature alternating, occurs oxidation reaction in the presence of residual oxygen in stove and consumes during alloy production.【4】VN alloy
The substantial amounts of gas for corroding sexual element containing sodium oxide molybdena, potassium oxide, sulfur dioxide etc. is produced in production process, corrosion graphite body
Bonding agent, causes graphite body to damage and consume.
In the past, technological staff was also directed to reducing the consumption of graphite body, the U of Chinese patent CN 205851874 always
A kind of cojoined graphite copple for being applied to production vanadium-nitrogen alloy product is disclosed, using the square unitary design of upper-thin-lower-thick, is protected
Uniform force, easy batch micro operations are demonstrate,proved；The U of Chinese patent CN 205784623 disclose a kind of sintering saggar system of VN alloy
Method is made, design method is connected with slide using slide bar, damaging body certain can be changed with corresponding, it is not necessary to be lost
Abandon, save cost；The U of Chinese patent CN 205851874 disclose a kind of sintering saggar manufacturer of combined type VN alloy
Method, using Combination Designs such as inserted sheet, neck and bases, also reduces consuming cost.
Document disclosed above is all the improvement from the structure of body body design to make it change and easy to maintenance, due to it
Material does not change, and oxidation and corrosive gas and body contact surface and contacts path and does not also change, and causes its service life
It inherently can not effectively be extended, be had much room for improvement.
The content of the invention
Present invention aims to overcome that there is provided a kind of anticorrosion, wear-resisting service life for the deficiency of above-mentioned prior art presence
Long sintering saggar of production VN alloy and preparation method thereof.
To realize the object of the invention, there is provided following technical scheme：One kind production VN alloy body protective layer, it is described
Protective layer is uniformly applied to the inside and outside layer surface of vanadium-nitrogen alloy sintering saggar, is mixed and made by solid powder and organic solvent
Into, it is characterised in that the component of solid powder includes 70 ~ 85wt% of mullite, 10 ~ 22wt% of carborundum, match by mass percentage
Grand 2.0 ~ 5.0wt% of ceramic powder, 0.5 ~ 2.0wt% of metallic aluminium powder, 0.5 ~ 2.0wt% of metallic silicon power；
The component of organic solvent includes liquid phenolic resin and absolute alcohol, and liquid phenolic resin and absolute alcohol are by weight percentage
Ratio be：70~90 wt%：10~30 wt%；
The ratio of solid powder and organic solvent agent by weight percentage is 100 wt%：30~50 wt%.
Preferably, solid powder by corresponding composition chemical analysis mass percent include Al2O3 49.75 ~
60.35wt%, SiO2 18.5~23.0 wt%, SiC10~22 wt%, SiALON 2.0~5.0 wt%, Al 0.5~2.0
The wt% of wt%, Si 0.5 ~ 2.0, surplus is inevitable impurity.
Preferably, the requirement of mullite, carborundum, Sialon ceramics Powder Particle Size is less than 200 mesh.
Preferably, metallic aluminium powder and metallic silicon power require≤325 mesh.Most preferably, metallic aluminium powder and metallic silicon power requirement
Equal to 325 mesh, this granularity is thinner than the granularity of other raw materials in product of the present invention, is more beneficial for matching grand solid solution fine particle
Generation, with more excellent anti-oxidant and erosion-resisting performance.Residual protective layer after to use carries out ore deposit scanning phase, it was confirmed that
Above-mentioned conclusion.
Preferably, mullite requirement：Al2O3 ≧71.0wt%, SiO2≤ 26.00 wt%, Zhen Bi Chong≤3.0, show
Qi Kong Shuai≤3.4%, mullite Xiang≤97.5wt%, surplus is inevitable impurity.Mullite is Al2O3- SiO2Binary system
Binary solid solution uniquely stable under middle normal pressure, with good high temperature resistant, wear-resistant, heat-resistant knocking stability.Compare in the present invention
Compared with a variety of refractory raw materials, comprehensive cost performance and using effect are optimal using mullite.
Preferably, carborundum requires SiC≤97.0wt%.Carborundum chemical property is particularly stable, antioxygenic property is excellent
More, thermal conductivity factor is high, thermal coefficient of expansion is small, anti-wear performance is good, and the present invention is screened through test of many times, chooses carborundum and is used as protection
One of layer main material, erosion, oxidation resistant effect are done to reach.
Sialon ceramics powder is the powder of Sialon ceramics, and Sialon ceramics has preferable toughness, very high hardness and wearability,
And unusual high high-temperature oxidation resistance, its main component is silicon, aluminium, oxygen and nitrogen, be silicon-aluminium-oxygen-nitrogen system and
The solid solution of its related substances system.
To realize that the object of the invention produces VN alloy body protective layer preparation method there is provided one kind, it is characterised in that
Comprise the following steps：
A. solid powder prepares：It is 70 ~ 85wt% of mullite, 10 ~ 22wt% of carborundum, Sialon ceramics powder 2.0 by mass percentage
~ 5.0wt%, 0.5 ~ 2.0wt% of metallic aluminium powder, 0.5 ~ 2.0wt% of metallic silicon power are mixed evenly that to obtain solid powder standby；
B. organic solvent prepares：By liquid phenolic resin and absolute alcohol by weight 70 ~ 90 wt%：10 ~ 30 wt% are well mixed
It is standby as organic solvent；
C. by the above-mentioned solid powder got ready by weight percentage 100：30 ~ 50 wt% add organic solvent, stir, and load
In sealed plastic barrel, as saggar protective layer finished product；
D. in use, opening Plastic Drum, stir, pulpous state saggar protective layer is uniformly applied to vanadium-nitrogen alloy sintering with brush
With the inside and outside layer surface of saggar, thickness control can be used in 0.5 ~ 1.0mm after spontaneously drying.
Key technology in the present invention is to introduce metallic aluminium powder and metallic silicon power.The particularity of vanadium-nitrogen alloy sintering technique,
Nitrogen is full of in burner hearth, but due to burner hearth intermittent feeding, discharge, causes a small amount of oxygen to enter, is also produced in reduction process a variety of
Corrosive gas, this causes graphite sintering saggar to be oxidized and corrode.It is well known that aluminium and silicon Wheat Protein, but
The present invention has found that metallic aluminium powder and metallic silicon power of the disperse in protective layer high temperature nitrogen in burner hearth are acted on by testing inspection
In, the grand particulate solid solution of generation match has just made the micropore produced by organic solvent Pintsch process up, has blocked oxidation or rotten
The passage of corrosion gas contact, so as to strengthen the protection to graphite sintering saggar.
Liquid phenolic resin is introduced in the present invention, because phenolic resin water-retention value is extremely low, there is good heat-resisting quantity, even if
At very high temperatures, the globality and stability of its structure can also be kept.It ensure that metallic aluminium powder and metallic silicon power exist
It is not oxidized in whole technique, a variety of aqueous solvents are once used in an experiment, cause protective layer effect to be had a greatly reduced quality.In an experiment
Also other anhydrous organic solvents are once used, effect is all preferable without phenolic resin.It is to adjust constructing for product to introduce absolute alcohol
Performance, after protective layer is coated, alcohol therein volatilizees soon to be finished.Attempt simply to be used as load using other anhydrous organic solvents
Body can not change the essence of the present invention.
Beneficial effect of the present invention：
1st, protect graphite to sinter body not to be corroded.When filling the sintering saggar of VN alloy green-ball in tunnel cave or push pedal
When being sintered in kiln, the protective layer is sintered together under high temperature and nitrogen atmosphere effect with graphite body, forms one layer
Fine and close protective layer, the passage for having blocked oxidizing gas or corrosive gas to be contacted with graphite body, so as to protect stone
Black matter sintering body is not oxidized or corrodes.
2nd, in body loading and removal VN alloy ball, the protective layer bears the impact and friction of material, protects
Graphite sintering body is not depleted.
3rd, the protective layer and graphite body are sintered together, and also improve the bulk strength of graphite body.
As a result product of the present invention shows that graphite sinters the use longevity of body after two VN alloy pushed bat kilns are on probation
Life averagely improves 28.6%, and cost averagely have dropped 18.82%.It is high through this protective layer is applied into VN alloy pushed bat kiln
It is also in use using three months on the graphite kiln-lining brick of temperature section, work well.
Embodiment
Below by way of specific embodiment, the present invention is further described.
Embodiment 1：
Feedstock analysis result is as follows：Mullite：Al2O3 71.05wt%, SiO226.41 wt%, true specific gravity 3.06, apparent pore
Rate 3.35%, mullite phase 97.78wt%.Carborundum：SiC 97.90wt%.
The raw materials such as mullite, carborundum, Sialon ceramics powder, metallic aluminium powder, metallic silicon power are carried out with 200 eye mesh screens respectively
Screening, extracting screen underflow is standby.It is mullite 85wt%, carborundum 12wt%, Sialon ceramics powder by mass percentage by above-mentioned raw materials
2.0wt%, metallic aluminium powder 0.5wt%, 100 kilograms of metallic silicon power 0.5wt% dispensings, the raw material prepared is mixed evenly and obtained
Sinter body protective layer solid powder.By liquid phenolic resin and absolute alcohol by weight 90 wt%：The well mixed systems of 10 wt%
Obtain organic solvent.Organic solvent made from adding 50 kilograms in the above-mentioned 100 kilograms of powders got ready, stirs, and loads close
Seal in Plastic Drum, that is, sintering saggar protective layer finished product is made.Pulpous state saggar protective layer, which will be made, with brush is uniformly applied to vanadium nitrogen
The inside and outside layer surface of alloy sintering saggar, measures thickness for 1.0mm, can be come into operation after spontaneously drying.
The chemical analysis of sintering body protective layer solid powder is by mass percentage made from detection：Al2O3
60.35wt%, SiO222.49 wt%, SiC 11.8 wt%, SiALON 2.0wt%, Al 0.5 wt%, the wt% of Si 0.5,
Surplus is impurity.
Embodiment 2：
Feedstock analysis result is as follows：Mullite：Al2O3 71.63wt%, SiO226.05 wt%, true specific gravity 3.02, apparent pore
Rate 3.38%, mullite phase 97.5wt%.Carborundum：SiC 97.0wt%.
The raw materials such as mullite, carborundum, Sialon ceramics powder, metallic aluminium powder, metallic silicon power are carried out with 200 eye mesh screens respectively
Screening, extracting screen underflow is standby.It is mullite 70wt%, carborundum 22wt%, Sialon ceramics powder by mass percentage by above-mentioned raw materials
5.0wt%, metallic aluminium powder 1.5wt%, 100 kilograms of metallic silicon power 1.5wt% dispensings, the raw material prepared is mixed evenly and obtained
Sinter body protective layer solid powder.By liquid phenolic resin and absolute alcohol by weight 80 wt%：The well mixed systems of 20 wt%
Obtain organic solvent.Organic solvent made from adding 40 kilograms in the above-mentioned 100 kilograms of powders got ready, stirs, and loads close
Seal in Plastic Drum, that is, sintering saggar protective layer finished product is made.Pulpous state saggar protective layer, which will be made, with brush is uniformly applied to vanadium nitrogen
The inside and outside layer surface of alloy sintering saggar, measures thickness for 0.8mm, can be come into operation after spontaneously drying.
The chemical analysis of sintering body protective layer solid powder is by mass percentage made from detection：Al2O3
50.64wt%, SiO2 19.16 wt%, SiC 21.3 wt%, SiALON 5.0wt%, Al 1.5 wt%, Si 1.5
Wt%, surplus is impurity.
Embodiment 3：
Feedstock analysis result is as follows：Mullite：Al2O3 71.55wt%, SiO226.6 wt%, true specific gravity 3.03, apparent pore
Rate 3.62%, mullite phase 97.53wt%.Carborundum：SiC 98.0wt%.
The raw materials such as mullite, carborundum, Sialon ceramics powder, metallic aluminium powder, metallic silicon power are carried out with 200 eye mesh screens respectively
Screening, extracting screen underflow is standby.It is mullite 75wt%, carborundum 18wt%, Sialon ceramics powder by mass percentage by above-mentioned raw materials
4.0wt%, metallic aluminium powder 2.0wt%, 100 kilograms of metallic silicon power 2.0wt% dispensings, the raw material prepared is mixed evenly and obtained
Sinter body protective layer solid powder.By liquid phenolic resin and absolute alcohol by weight 70 wt%：The well mixed systems of 30 wt%
Obtain organic solvent.Organic solvent made from adding 30 kilograms in the above-mentioned 100 kilograms of powders got ready, stirs, and loads close
Seal in Plastic Drum, that is, sintering saggar protective layer finished product is made.Pulpous state saggar protective layer, which will be made, with brush is uniformly applied to vanadium nitrogen
The inside and outside layer surface of alloy sintering saggar, measures thickness for 0.5mm, can be come into operation after spontaneously drying.
The chemical analysis of sintering body protective layer solid powder is by mass percentage made from detection：Al2O3
53.69wt%, SiO219.98 wt%, SiC 17.6 wt%, SiALON 4.0wt%, Al 2.0 wt%, the wt% of Si 2.0,
Surplus is impurity.
Claims (7)
1. one kind production VN alloy body protective layer, the protective layer is uniformly applied in vanadium-nitrogen alloy sintering saggar
Superficies, are mixed by solid powder and organic solvent and are made, it is characterised in that the component of solid powder presses quality percentage
Than meter include 70 ~ 85wt% of mullite, 10 ~ 22wt% of carborundum, 2.0 ~ 5.0wt% of Sialon ceramics powder, metallic aluminium powder 0.5 ~
2.0wt%, 0.5 ~ 2.0wt% of metallic silicon power；
The component of organic solvent includes liquid phenolic resin and absolute alcohol, and liquid phenolic resin and absolute alcohol are by weight percentage
Ratio be：70~90 wt%：10~30 wt%；
The ratio of solid powder and organic solvent agent by weight percentage is 100 wt%：30~50 wt%.
2. a kind of production VN alloy body protective layer according to claim 1, it is characterised in that solid powder presses phase
Constitutional chemistry composition mass percent is answered to include the wt% of Al2O3 49.75 ~ 60.35wt%, SiO2 18.5 ~ 23.0, SiC10 ~ 22
Wt%, SiALON 2.0 ~ 5.0 wt%, Al 0.5 ~ 2.0 wt%, Si 0.5 ~ 2.0 wt%, surplus are inevitable impurity.
3. a kind of production VN alloy body protective layer according to claim 1, it is characterised in that mullite, carbonization
Silicon, the requirement of Sialon ceramics Powder Particle Size are less than 200 mesh.
4. a kind of production VN alloy body protective layer according to claim 1, it is characterised in that metallic aluminium powder and gold
Belong to silica flour and require≤325 mesh.
5. a kind of production VN alloy body protective layer according to claim 1, it is characterised in that mullite requirement：
Al2O3 ≧71.0wt%, SiO2≤ 26.00 wt%, Zhen Bi Chong≤3.0, Xian Qi Kong Shuai≤3.4%, mullite Xiang≤
97.5wt%, surplus is inevitable impurity.
6. a kind of production VN alloy body protective layer according to claim 1, it is characterised in that carborundum requires SiC
≧97.0wt%。
7. a kind of production VN alloy body protective layer preparation method as described in one of claim 1 ~ 6, it is characterised in that
Comprise the following steps：
A. solid powder prepares：It is 70 ~ 85wt% of mullite, 10 ~ 22wt% of carborundum, Sialon ceramics powder 2.0 by mass percentage
~ 5.0wt%, 0.5 ~ 2.0wt% of metallic aluminium powder, 0.5 ~ 2.0wt% of metallic silicon power are mixed evenly that to obtain solid powder standby；
B. organic solvent prepares：By liquid phenolic resin and absolute alcohol by weight 70 ~ 90 wt%：10 ~ 30 wt% are well mixed
It is standby as organic solvent；
C. by the above-mentioned solid powder got ready by weight percentage 100：30 ~ 50 wt% add organic solvent, stir, and load
In sealed plastic barrel, as saggar protective layer finished product；
D. in use, opening Plastic Drum, stir, pulpous state saggar protective layer is uniformly applied to vanadium-nitrogen alloy sintering with brush
With the inside and outside layer surface of saggar, thickness control can be used in 0.5 ~ 1.0mm after spontaneously drying.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675780A (en) * | 2018-06-11 | 2018-10-19 | 郑州大学 | A kind of metal composite mullite silicon carbide ceramic composite and preparation method thereof |
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| US20040157724A1 (en) * | 2003-02-07 | 2004-08-12 | Doza Douglas K. | Crack-resistant insulating dry refractory |
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| CN203657450U (en) * | 2013-11-27 | 2014-06-18 | 陕西丰源钒业科技发展有限公司 | Nitridation sintering section device for producing vanadium-nitrogen alloy by means of one-step method and double pushed slab kiln |
| CN106187247A (en) * | 2016-07-26 | 2016-12-07 | 唐山贝斯特高温材料有限公司 | Metallic aluminium silicon carbide composite diphase material and preparation method thereof |
| EP3191429A1 (en) * | 2014-09-11 | 2017-07-19 | Refratechnik Holding GmbH | Batch for a product fired from reaction-bonded silicon carbide, use of the batch, and a refractory product consisting of said batch |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040157724A1 (en) * | 2003-02-07 | 2004-08-12 | Doza Douglas K. | Crack-resistant insulating dry refractory |
| CN201664605U (en) * | 2010-04-08 | 2010-12-08 | 江阴市长兴钒氮新材料有限公司 | Sagger special for vanadium nitrogen alloy |
| CN203657450U (en) * | 2013-11-27 | 2014-06-18 | 陕西丰源钒业科技发展有限公司 | Nitridation sintering section device for producing vanadium-nitrogen alloy by means of one-step method and double pushed slab kiln |
| EP3191429A1 (en) * | 2014-09-11 | 2017-07-19 | Refratechnik Holding GmbH | Batch for a product fired from reaction-bonded silicon carbide, use of the batch, and a refractory product consisting of said batch |
| CN106187247A (en) * | 2016-07-26 | 2016-12-07 | 唐山贝斯特高温材料有限公司 | Metallic aluminium silicon carbide composite diphase material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675780A (en) * | 2018-06-11 | 2018-10-19 | 郑州大学 | A kind of metal composite mullite silicon carbide ceramic composite and preparation method thereof |
| CN108675780B (en) * | 2018-06-11 | 2021-08-24 | 郑州大学 | Metal composite mullite-silicon carbide ceramic composite material and preparation method thereof |
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| CN107311697B (en) | 2020-11-06 |
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