CN100423873C - Preparation method of TiB2 nanometer micrometer structure feeding for hot spraying - Google Patents
Preparation method of TiB2 nanometer micrometer structure feeding for hot spraying Download PDFInfo
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- CN100423873C CN100423873C CNB200610113293XA CN200610113293A CN100423873C CN 100423873 C CN100423873 C CN 100423873C CN B200610113293X A CNB200610113293X A CN B200610113293XA CN 200610113293 A CN200610113293 A CN 200610113293A CN 100423873 C CN100423873 C CN 100423873C
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Abstract
The invention relates to a method for preparing TiB2 nanometer-micrometer feeding material used in thermal plating. Wherein, it mixes TiB2 powder whose diameter granularity is lower than 5 mum with other nanometer particles whose granularity is lower than 0.2 mum; uses wet ball grinding method and ultrasonic wave treatment to obtain nanometer-micrometer suspension; then atomizes and dries said suspension to obtain the group powder of TiB2 nanometer-micrometer structure; then thermally vacuuming the group powder to obtain said TiB2 nanometer-micrometer feeding. The inventive feeding has ball shape, uniform granularity, and flowability at 60-102s/50g.
Description
Technical field:
A kind of used for hot spraying TiB
2The preparation method of nanometer micrometer structure feeding belongs to the powder manufacture field.
Background technology:
TiB
2Having high-melting-point, high rigidity, low-density, many excellent properties such as resistance to chemical corrosion that wearability is good, high, is continue WC, Cr
3C
2High-temperature wearable oxidation-resistant material afterwards is widely used in fields such as Aero-Space, weaponry, metallurgy, cutter.Become the focus material of thermal spraying Research on Surface Modification.Synthetic (SHS) method of self propagating high temperature is domestic and international industrial production high-purity Ti B at present
2The main mode of powder.But the powder particle out-of-shape that this mode is produced, particle diameter is tiny, and particle size distribution is at 0.1～5.0 μ m, and is mobile poor, and powder feeding is very difficult in the hot-spraying technique.
From thermal spraying TiB
2The research history of ceramic coating, TiB
2Normal vacuum plasma spray coating or the low-voltage plasma spraying of adopting, these two kinds of spraying methods are with high costs, and limited by vacuum-chamber dimensions, can not spray bulk specimen.Adopting air plasma spraying then is the mode of less expensive, yet under atmospheric conditions, TiB
2Easy oxidation and flying speed in the high-temperature plasma line are little, and the kinetic energy of bump matrix is low, and it is poor with combining of matrix to cause, and deposition efficiency is low, the coating porosity height.These unfavorable factors obviously influence coating quality and coatings applications.
Studies show that in recent years, 1) TiB
2Suitably select additive in the hot spray powder, can improve coating quality.Add the oxidation kinetics characteristic that SiC at high temperature can change boride ceramics in the thermal spraying boride powder, hinder its oxidation product B
2O
3Vaporization at high temperature, make B
2O
3Initial volatilization temperature bring up to 1400K from 700K; MoSi
2As additive, in coating as TiB
2The bonding phase, make the coating densification.2) hot-spraying nano structural ceramics coating has the incomparable excellent performance of the conventional ceramic coating of thermal spraying.The ceramic nano structure coating of thermal spraying preparation, porosity is low, and wearability improves, and toughness improves, and fragility descends.And nanometer powder can not be directly used in thermal spraying.It is the mode that thermal spraying prepares the simple and fast of nano-structured coating that nanometer powder is reconstituted micron powder, is the main flow mode that current domestic and international thermal spraying prepares nano-structured coating.Thereby, select suitable additive, preparation is fit to the TiB of thermal spraying
2Powder is to obtain high-quality thermal spraying TiB
2The prerequisite of coating.The spray drying granulation product is in grain shape, and particle diameter distributes, and aspects such as flowability can satisfy the physical property requirement of thermal spraying to powder, spray dried products is heat-treated the organic active agent that effectively to remove in the powder, but in the atmosphere heating furnace, under the hot conditions, TiB
2Powder meeting oxidation, vacuum heat can effectively suppress oxidation, guarantees TiB
2Powder pure, vacuum high-temperature is still preserved the part nano-scale particle after handling in the particle.Select suitable spraying parameter, thermal spraying TiB
2Nanometer micrometer structure feeding is expected to obtain the coating of nanostructured.
Summary of the invention:
The purpose of this invention is to provide a kind of used for hot spraying TiB
2The preparation method of nanometer micrometer structure feeding, the TiB that makes preparation
2The nanometer micrometer structure feeding particle diameter is even, and good fluidity is applicable to thermal spraying.
In order to obtain to be fit to the TiB of thermal spraying
2Nanometer micrometer structure feeding, the present invention has adopted following steps:
1), with the submicron order TiB of particle mean size less than 5 μ m
2Powder or nanoscale TiB
2Powder and granularity are less than nano grade Sic, the MoSi of 0.2 μ m
2, Al
2O
3, MgO, ZrO
2One or more by (97～60): (3～40) mass ratio carries out batch mixing, adds surfactant behind the batch mixing, and the 20KHz ultrasonic wave is handled 15min and obtained to receive a micron suspension behind the wet ball grinding 1.5h;
2), adopt 50～75 ℃ of chargings of suspension constant temperature, 210～240 ℃ inlet temperature, feeding speed is controlled at 2～4L/hr, the centrifugal pan rotating speed is controlled at 20000～35000r/min spray-drying suspension, obtains TiB
2The reunion powder of nanometer micrometer structure;
3) place vacuum to be higher than 10 in spray-dired reunion powder
-3In the Vacuum diffusion bonding furnace of Pa, 1200～1400 ℃ of heat treatment temperatures are incubated 1.5～2.5 hours, with the stove cooling, obtain used for hot spraying TiB
2Nanometer micrometer structure feeding.
Described surfactant is one of polyvinyl alcohol, polyethylene glycol, polyacrylic acid ammonia, tributyl phosphate, carboxymethyl cellulose, and content is less than 45g/L in the suspension.
Efficient wet ball milling and ultrasonic wave are handled to such an extent that main purpose is to obtain single-phase or heterogeneous finely dispersed suspension.
Adopt 50～75 ℃ of heating of water bath with thermostatic control suspension in the spray-drying feeding process, can reduce the temperature difference between hot-air and liquid material, improve water evaporates efficient, obtain the high reunion powder of sphericity.By spray drying treatment, TiB
2The particle size range of reunion powder is at 5～75 μ m.
The purpose of vacuum heat is to remove the residual moisture and the surfactant of spray-drying reunion powder, purifying reunion powder; At high temperature merge between the nano particle of agglomerated powder particles inside simultaneously, improve the compactness of reunion powder, select proper heat treatment temperature and temperature retention time, the inner nano particle of reunion powder particles still keeps nano-scale.
Utilize the used for hot spraying TiB of method preparation of the present invention
2Nanometer micrometer structure feeding, its powder granule outward appearance are spherical, and even particle size distribution, size are between 5～75 μ m, and single spheric granules inside still keeps existing nano particle.Handle the powder that can obtain the different grain size distribution through vibrosieve, its flowability satisfies the physical property requirement of thermal spraying to powder at 60～102s/50g.
Description of drawings
Fig. 1 utilizes the TiB of the inventive method preparation
2/ Al
2O
3The pattern that nanometer micrometer structure feeding is observed under SEM.
Fig. 2 utilizes the TiB of the inventive method preparation
2The pattern that/SiC nanometer micrometer structure feeding is observed under SEM;
Fig. 3 utilizes the TiB of the inventive method preparation
2The surface topography of the individual particle that/SiC nanometer micrometer structure feeding is observed under high resolution scanning electron microscope.
The specific embodiment
Embodiment 1:TiB
2/ Al
2O
3The preparation of nanometer micrometer structure feeding
Get the TiB of granularity less than 5 μ m
2Powder 250g, particle size range is the Al of 80～200nm
2O
3Powder 50g mixes, and carries out ball milling, and ball-milling medium is a deionized water, adds and contains the deionized water solution that the surfactant quality is 23g, is mixed with the slip that volume is 1L, and ball milling 1.5hr in the high-efficiency vertical ball mill handles 15min with the ultrasonic wave of 20KHz again.Be mixed with suspension like this with certain viscosity.The suspension that spray-drying has prepared in high speed electric centrifugal spray drying equipment.The spray-drying parameter is chosen as: 240 ℃ of temperature of inlet air, outlet temperature are 120 ℃; 50 ℃ of heating of water bath with thermostatic control suspension in the spray-drying feeding process, feeding speed is controlled at 4L/hr, and the centrifugal pan rotating speed is controlled at 35000r/min. by spray drying treatment, can obtain the TiB of 5～75 μ m
2/ Al
2O
3The reunion powder.The heat treatment in Vacuum diffusion bonding furnace of reunion powder, vacuum are 10
-3Pa, heat treatment temperature is 1200 ℃, is incubated 1.5 hours, with the stove cooling, can obtain TiB
2/ Al
2O
3Nanometer micrometer structure feeding.
Under SEM, observe its pattern, the shape approximation sphere of the powder of as can be seen from Figure 1 reuniting, particle size distribution is between 5～75 μ m.Utilize the vibrosieve classification to handle and obtain the reunion powder of size distribution at 15～45 μ m, mobile with the test of Hall mobility-detected instrument, the flowing time of 50g powder is 96～98s; Size distribution is at the reunion powder of 45～75 μ m, and the flowing time of 50g powder is 60～63s.
Embodiment 2:TiB
2The preparation of/SiC nanometer micrometer structure feeding
Get the TiB of granularity less than 5 μ m
2Powder 240g, particle diameter mixes less than the SiC powder 160g of 80nm, carry out ball milling 1hr, ball-milling medium is a deionized water, add again and contain the deionized water solution that the surfactant quality is 32g, be mixed with the slip that volume is 1L, ball milling 1.5hr in the high-efficiency vertical ball mill handles 15min with the ultrasonic wave of 20KHz again.Be mixed with suspension like this with certain viscosity.The suspension that spray-drying has prepared in high speed electric centrifugal spray drying equipment.The spray-drying parameter is chosen as: 210 ℃ of temperature of inlet air, outlet temperature are 130 ℃; 75 ℃ of heating of water bath with thermostatic control suspension in the spray-drying feeding process, feeding speed is controlled at 2L/hr, and the centrifugal pan rotating speed is controlled at 25000r/min. by spray drying treatment, can obtain the TiB of 5～75 μ m
2/ SiC reunion powder.The heat treatment in Vacuum diffusion bonding furnace of reunion powder, vacuum are 10
-3Pa, heat treatment temperature is 1400 ℃, is incubated 2.5 hours, with the stove cooling, can obtain TiB
2The nanometer micrometer structure feeding of/SiC.
Under SEM, observe its pattern, the shape approximation sphere of the powder of as can be seen from Figure 2 reuniting, particle size distribution is between 5～75 μ m.Utilize the vibrosieve classification to handle and obtain the reunion powder of size distribution at 15～45 μ m, mobile with the test of Hall mobility-detected instrument, the flowing time of 50g powder is 101～102s.Size distribution is at the reunion powder of 45～75 μ m, and the flowing time of 50g powder is 76～78s.
More than the analysis showed that the used for hot spraying TiB of method preparation of the present invention
2Receive (little) rice structure feeding, its powder granule outward appearance is spherical, and even particle size distribution, size are between 5～75 μ m, and single spheric granules inside still keeps existing nano particle, sees accompanying drawing 3.Handle the powder that can obtain the different grain size distribution through vibrosieve, its flowability satisfies the physical property requirement of thermal spraying to powder at 60～102s/50g.
Claims (2)
1. used for hot spraying TiB
2The preparation method of nanometer micrometer structure feeding is characterized in that, has adopted following steps:
1), with the submicron order TiB of particle mean size less than 5 μ m
2Powder or nanoscale TiB
2Powder and granularity are less than nano grade Sic, the MoSi of 0.2 μ m
2, Al
2O
3, MgO, ZrO
2One or more by 97～60: 3～40 mass ratioes carry out batch mixing, add surfactant behind the batch mixing, and the 20KHz ultrasonic wave is handled 15min and obtained to receive a micron suspension behind the wet ball grinding 1.5h;
2), adopt 50～75 ℃ of chargings of suspension constant temperature, 210～240 ℃ inlet temperature, feeding speed is controlled at 2～4L/hr, the centrifugal pan rotating speed is controlled at 20000～35000r/min spray-drying suspension, obtains TiB
2The reunion powder of nanometer micrometer structure;
3) place vacuum to be higher than 10 in spray-dired reunion powder
-3In the Vacuum diffusion bonding furnace of Pa, 1200～1400 ℃ of heat treatment temperatures are incubated 1.5～2.5 hours, with the stove cooling, obtain used for hot spraying TiB
2Nanometer micrometer structure feeding.
2. a kind of used for hot spraying TiB according to claim 1
2The preparation method of nanometer micrometer structure feeding is characterized in that, described surfactant is one of polyvinyl alcohol, polyethylene glycol, polyacrylic acid ammonia, tributyl phosphate, carboxymethyl cellulose, and the content in suspension is less than 45g/L.
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| CNB200610113293XA CN100423873C (en) | 2006-09-22 | 2006-09-22 | Preparation method of TiB2 nanometer micrometer structure feeding for hot spraying |
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|---|---|---|---|
| CNB200610113293XA CN100423873C (en) | 2006-09-22 | 2006-09-22 | Preparation method of TiB2 nanometer micrometer structure feeding for hot spraying |
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| CN100423873C true CN100423873C (en) | 2008-10-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3194096A4 (en) * | 2014-09-18 | 2018-05-02 | Oerlikon Metco (US) Inc. | Pre-formulated powder feedstock |
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| CN101200282B (en) * | 2007-12-12 | 2010-06-30 | 四川大学 | Vacuum heat-treating method for nano powder |
| CN102021587B (en) * | 2010-12-03 | 2012-05-30 | 湖北工业大学 | AL2O3 plus TiB2 plus Al composite coating formed by reaction spray coating on surface of aluminum alloy and stirring friction welding and preparation method thereof |
| CN102581292A (en) * | 2012-03-13 | 2012-07-18 | 北京工业大学 | Preparation method of coating containing TiB2 metal ceramic composite powder for thermal spraying piston ring |
| CN103074565A (en) * | 2012-12-11 | 2013-05-01 | 北矿新材科技有限公司 | Preparation method of solid oxide electrolytic cell connector coating spraying powder |
| CN103011828A (en) * | 2012-12-27 | 2013-04-03 | 北京工业大学 | Preparation method of agglomerated composite thermal spraying powder of boride-containing ceramic |
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| CN103601499A (en) * | 2013-11-04 | 2014-02-26 | 天津大学 | Method for preparing TiB2 (titanium diboride) nano powder by using sol-gel technique |
| CN105695917A (en) * | 2016-03-24 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | High-temperature and ablation resistance TiB2-MoSi2 composite coating and preparation method thereof |
| CN108393484B (en) * | 2018-02-06 | 2020-08-18 | 广东正德材料表面科技有限公司 | Metal ceramic nano composite structure feed for thermal spraying and preparation method thereof |
| CN108441808B (en) * | 2018-06-21 | 2020-01-14 | 江西科技师范大学 | Preparation method of cathode titanium diboride coating for aluminum electrolytic cell |
| CN110045549B (en) * | 2019-03-22 | 2023-12-26 | 湖南飞优特电子科技有限公司 | LCD powder cluster bad control device |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4327186A (en) * | 1980-06-23 | 1982-04-27 | Kennecott Corporation | Sintered silicon carbide-titanium diboride mixtures and articles thereof |
| CN1152562A (en) * | 1996-10-30 | 1997-06-25 | 大连理工大学 | Method of preparing (AlxOx+TiBx) foamed ceramic filter by self-overgrowth high-temp. synthesis control |
| US5837326A (en) * | 1996-04-10 | 1998-11-17 | National Research Council Of Canada | Thermally sprayed titanium diboride composite coatings |
| JP2001146474A (en) * | 1999-11-15 | 2001-05-29 | Kubota Corp | Ceramic sintered compact of titanium diboride and production method |
| CN1371863A (en) * | 2002-04-01 | 2002-10-02 | 武汉理工大学 | Process for preparing titanium diboride nano powder |
| CN1453243A (en) * | 2003-05-29 | 2003-11-05 | 上海交通大学 | Prepn of large grain spherical submicron/nano composite fiber-ceramic powder |
| US20040258916A1 (en) * | 2002-12-12 | 2004-12-23 | Centro Sviluppo Materiali S.P.A. | Silicon carbide-based thermal spray powder, method of preparation and use |
| CN1600820A (en) * | 2003-09-25 | 2005-03-30 | 中国科学院金属研究所 | Preparation of thermal spraying powder in use for nano abrasion resistant coating and use |
| CN1793058A (en) * | 2005-11-10 | 2006-06-28 | 上海交通大学 | Process for preparing large particle spherical metal ceramic nano composite spraying powder |
-
2006
- 2006-09-22 CN CNB200610113293XA patent/CN100423873C/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4327186A (en) * | 1980-06-23 | 1982-04-27 | Kennecott Corporation | Sintered silicon carbide-titanium diboride mixtures and articles thereof |
| US5837326A (en) * | 1996-04-10 | 1998-11-17 | National Research Council Of Canada | Thermally sprayed titanium diboride composite coatings |
| CN1152562A (en) * | 1996-10-30 | 1997-06-25 | 大连理工大学 | Method of preparing (AlxOx+TiBx) foamed ceramic filter by self-overgrowth high-temp. synthesis control |
| JP2001146474A (en) * | 1999-11-15 | 2001-05-29 | Kubota Corp | Ceramic sintered compact of titanium diboride and production method |
| CN1371863A (en) * | 2002-04-01 | 2002-10-02 | 武汉理工大学 | Process for preparing titanium diboride nano powder |
| US20040258916A1 (en) * | 2002-12-12 | 2004-12-23 | Centro Sviluppo Materiali S.P.A. | Silicon carbide-based thermal spray powder, method of preparation and use |
| CN1453243A (en) * | 2003-05-29 | 2003-11-05 | 上海交通大学 | Prepn of large grain spherical submicron/nano composite fiber-ceramic powder |
| CN1600820A (en) * | 2003-09-25 | 2005-03-30 | 中国科学院金属研究所 | Preparation of thermal spraying powder in use for nano abrasion resistant coating and use |
| CN1793058A (en) * | 2005-11-10 | 2006-06-28 | 上海交通大学 | Process for preparing large particle spherical metal ceramic nano composite spraying powder |
Non-Patent Citations (2)
| Title |
|---|
| 喷雾干燥YPSZ纳米结构热喷涂粉末材料制备及表征. 林锋，蒋显亮，任先京，李振铎，周恒，崔颖.功能材料，第36卷第11期. 2005 |
| 喷雾干燥YPSZ纳米结构热喷涂粉末材料制备及表征. 林锋，蒋显亮，任先京，李振铎，周恒，崔颖.功能材料，第36卷第11期. 2005 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3194096A4 (en) * | 2014-09-18 | 2018-05-02 | Oerlikon Metco (US) Inc. | Pre-formulated powder feedstock |
| US10329656B2 (en) | 2014-09-18 | 2019-06-25 | Oerlikon Metco (Us) Inc. | Pre-formulated powder feedstock |
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