CN105271750A - Preparation of enamel coating modified by rare earth doping and nanometer effect - Google Patents
Preparation of enamel coating modified by rare earth doping and nanometer effect Download PDFInfo
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Abstract
The performance of enamel is influenced by material composition, preparation technology, component granularity, etc. A mixture of rare earth oxide and nanometer silica is doped according to a certain ratio and the functions of activation and modification of the rare earth oxide are performed so as to facilitate reduction in firing temperature of the enamel, improvement of suspendability of glaze slip, buffering of thermal stress of the enamel, densification of porcelain glaze, etc.; and nanometer silica has high chemical activity and can obviously improve the integrity of a silicate network structure. Through cooperative effect of the rare earth oxide and nanometer silica, the prepared enamel coating has excellent overall performance and can meet performance demands in fields like modern industry and national defense. An optimal doping ratio of 96% of a glaze block, 3% of the rare earth oxide and 1% of the nanometer silica (SiO2) is obtained through experiment and exploration; and the prepared enamel coating has a uniform and compact surface, good adhesion, good bending resistance and substantially improved stability to acid chemicals, heat resistance, thermal shock resistance and shock strength. The matrix glaze of the enamel comprises zinc oxide, silica, alumina, titanium oxide, nickel oxide, cobalt nitrate, phosphoric pentoxide, calcium fluoride, boric acid and sodium carbonate and is prepared through melting at 1150 to 1250 DEG C.
Description
Technical field
The present invention relates to a kind of matrix material and preparation method thereof, be specifically related to industrial enamel matrix material and preparation method thereof, belong to technical field of composite materials.
Background technology
Enamel is that unorganic glass material is coagulated a kind of matrix material on matrix metal and together with metal mortise by melting.Enamel is mainly used in steel plate, cast iron or aluminum products surface, so as to improving outward appearance, and protection metallic surface.Enamel is as the protective coating of metallic surface, and in machinery, metallurgy, each industry such as building, electronics, light industry, instrument and defense sector and even agricultural and people's daily life, Metal Surface Modification Technique has purposes widely.Therefore, constantly study the over-all properties that new Method and Technology improves enamel, extend the work-ing life of metallic substance, broaden application field has theoretical significance and actual application value.In a kind of prior art, select existing high-hardness corrosion-resistant enamel as matrix enamel, the composition of enamel matrix glaze has zinc oxide, silicon-dioxide, aluminum oxide, titanium oxide, nickel oxide, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, Vanadium Pentoxide in FLAKES, Calcium Fluoride (Fluorspan), boric acid, sodium carbonate, by the raw material after mixing, be placed on and be incubated 30min at 700 DEG C to remove moisture content in raw material and gas, then at 1200 ~ 1300 DEG C, 1.5h is founded, the glaze of melting is poured in cold water quench broken, 200 orders are milled to after drying, obtained glaze slip is sprayed on matrix steel plate after treatment, 5min is sintered at 950 DEG C.It has high rigidity and good acid resistance, but thermotolerance and thermal shock strength deficiency.
Summary of the invention
The object of the invention is, a kind of method improving enamel over-all properties is simply and effectively provided, extend enamelware and industrial equipments work-ing life, widen the Application Areas of enamel coating.Nano silicon has higher chemically reactive, and the appropriate nano silicon introduced can partly enter in the network structure of vitreous enamel, obviously can improve the integrity of silicate network structure, significantly improve the acid-resistant chemical stability of enamel coating.The doping of rare earth oxide can improve the heat-resisting acute degeneration of enamel and shock strength, improves glaze slip rheological property, reduces enamel firing temperature, improves enamel surfaces glossiness, strengthens adherence, reduces cold quick-fried and fish scale generation.Research shows, adding of rare earth oxide has no significant effect the acid-resistant chemical stability of enamel, by introducing the nano silicon of suitable proportion and the blending ingredients of rare earth oxide, utilizing its complementary and synergistic effect, significantly can improve the over-all properties of enamel.
According to an aspect of the present invention, provide a kind of preparation method of industrial enamel matrix material, the method comprises to grind the mixture that the mode added introduces a certain proportion of nano silicon and rare earth oxide simultaneously in vitreous enamel, and comprises the following steps:
A) weighing step, raw materials weighing, mixes;
B) drying step, is placed in loft drier dry 1.5 hours by the raw material mixed, to remove moisture in raw material and gas;
C) high temperature melting step, puts into crucible by raw material complete for drying, is at high temperature incubated, until wire drawing is without node;
D) quenching Step, is quickly cooled to room temperature by the raw material after fusing, obtain quenching broken after frit, then dry;
E) ball milling pulping stage, is broken into powder by dried frit ball milling powder, and the mixture weighing rare earth oxide and nanometer grade silica adds additive as mill, is milled to 200 orders after mixing.
According to a further aspect of the present invention, above-mentioned rare earth oxide is at least one selected from cerium oxide and lanthanum trioxide.
Accompanying drawing explanation
Figure 1A and 1B shows the surperficial metallograph of prior art glaze block enamel coating.
Fig. 2 A and 2B shows the surface of the enamel coating after according to mixed with nano-silicon dioxide of the present invention and cerium oxide metallograph.
Fig. 3 A and 3B respectively illustrates the enamel cross-sectional scans electromicroscopic photograph of the sample of Figure 1A-1B and Fig. 2 A-2B.
Fig. 4 is the X-ray diffraction spectrogram of the enamel coating material according to enamel coating material of the present invention and prior art.
Embodiment
According to the present invention, provide a kind of preparation method of industrial enamel matrix material, the method comprises to grind the mixture that the mode added introduces a certain proportion of nano silicon and rare earth oxide (cerium oxide or lanthanum trioxide) simultaneously in vitreous enamel, and comprises the following steps:
(1) weighing: raw materials weighing, mixes;
(2) dry: dry 1.5 hours (h) of the loft drier raw material mixed being placed in 700 ~ 800 DEG C, to remove moisture in raw material and gas;
(3) high temperature melting: raw material complete for drying is put into crucible, is incubated 1.5h at 1200 ~ 1300 DEG C, until wire drawing is without node;
(4) quench: the raw material after fusing is dropped in cold water immediately, is quickly cooled to room temperature, obtain quenching broken after frit, then dry;
(5) ball milling slurrying: dried frit ball milling powder is broken into powder, the mixture weighing rare earth oxide and nanometer grade silica (being respectively 3 ~ 6%wt, 1 ~ 4%wt) adds additive as mill, consisting of of glaze block and additive:
Glaze block: 90 ~ 96%,
Rare earth oxide: 3 ~ 6%,
Nano silicon: 1 ~ 4%,
200 orders are milled to after mixing; Airtight ageing 24h after adding appropriate alcohol;
(6) spray: with spray gun, glaze slip is uniformly sprayed on steel plate, and at 100 DEG C dry 1.5h;
(7) fire: dried steel plate is put in retort furnace, fire at 900 ~ 950 DEG C 5 ~ 7 minutes (min).
Below by way of concrete embodiment the present invention made and further illustrating
The preparation of this high-performance enamel comprises following processing step:
(1) weighing, dry: after being mixed in following ratio weighing by frit Raw Materials, to put into 750 DEG C of loft drier, dry 1.5h, to remove the moisture content in raw material, release gas;
Material consists of: zinc oxide 7%, silicon-dioxide 42.5%, aluminum oxide 5.7%, titanium oxide 2%, nickel oxide 2.5%, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 3.9%, Vanadium Pentoxide in FLAKES 2.4%, Calcium Fluoride (Fluorspan) 3.9%, boric acid 33.7%, sodium carbonate 27.4%;
(2) high temperature melting: raw material complete for drying is put into crucible, is incubated 1.5h at 1200 ~ 1300 DEG C, until wire drawing is without node, puts into cold water immediately and quench broken after taking-up.Then dry;
(3) ball milling slurrying: first glaze block is ground into Powdered after be divided into two parts, portion adds 3% cerium dioxide, the mixture of 1% silicon-dioxide, portion does not add any mill addition, the ratio being 25:1 in ball material weight ratio adds corundum abrading-ball in ball grinder, and grinding 24h, crosses 200 mesh sieves, add suitable alcohols, standing 24h makes it aging;
(4) to size mixing and the application of slip: in the glaze slip after aging, add raw spirit, till making it spray.With spray gun, glaze slip is uniformly sprayed on steel plate (2cr13 stainless steel, 30 × 40mm), makes its thickness reach 0.2 ~ 0.8mm, and at 100 DEG C dry 1.5h;
(5) fire: dried application of slip sample is put into retort furnace, at 930 DEG C, fires 7min, then taking-up is placed on asbestos plate and is cooled to room temperature;
Following test is carried out to the enamel of gained, and analyzes:
Acid resistance is tested: record the enamel coating citric acid of resistance to room temperature grade (1 grade is best, and less than 2 grades defective) according to GB GB/T9989-2005, record the acid fastness of enamel coating according to GB4738.2-84.
Micro-hardness testing: the hardness measuring enamel layer with the digital microhardness instrument of FVM-800, load 50gf, load time is 10s.
Thermotolerance and resistance to sudden heating test: measure enamel resistance toheat according to GB11418-2008, GB11419-2008 measures enamel layer heatproof acute degeneration.
Shock strength is tested: impact strength adopts ball falling impact method.Face up enamel horizontal positioned, does freely falling body clash into enamel coating with 50g steel ball directly over sample, observes the de-porcelain situation in surface, if without de-porcelain, increases and highly continue to clash into till de-porcelain.
Counter-bending test: according to GB/T6742-1986 GB, when test is bending, enamel coating is at cracking with from the stripping situation matrix.
Result is as following table 1:
Table 1 enamel coating all-round property testing
From above-mentioned contrast, its over-all properties of enamel coating after rare earth doped oxide compound according to the abovementioned embodiments of the present invention and nano silicon mixture makes moderate progress, and especially resistance to impact shock, thermal shock temperature and acid proof raising are the most remarkable.
The present inventor has carried out coating structure morphology analysis to the enamel that this embodiment obtains, that is: observe the tissue topography of enamel layer with LeikaDM4000M metaloscope and Quanta250FEG type environmental scanning electron microscope.Result is presented in Fig. 2 A-2B, Fig. 3 B.
As can be seen from the contrast of the metallograph of Figure 1A-1B, Fig. 2 A-2B, in the sample after rare earth doped oxide compound according to the abovementioned embodiments of the present invention and nano silicon mixture (Fig. 2 A and 2B), enamel surfaces is more even, fine and close; Because adding of rare earth makes Minute pores in enamel increase, the existence of this micropore makes the thermal stresses of enamel be cushioned, and stress and elasticity increase, so resistance to impact shock and heat-resisting acute degeneration improve.Because the part nano silicon added is not dissolved in enamel completely, and be present in enamel surfaces, thus chemical stability is more excellent; Appropriate nano silicon has no significant effect enamel luster performance.
Fig. 3 A and 3B respectively illustrates enamel cross-sectional scans Electronic Speculum (SEM) photo of the sample of Figure 1A-1B and Fig. 2 A-2B.From Fig. 3 A and 3B relatively, finer and close according to the enamel coating of mixed with nano-silicon dioxide of the present invention and rare earth oxide, and enamel coating is that dentation is combined with the bonding interface place of matrix; And the enamel coating compactness of prior art is poor, bonding surface interface opposed flattened; As can be seen here, to carry out the enamel coating bonding properties of modification by mixed with nano-silicon dioxide and rare earth oxide better according to of the present invention.
Fig. 4 is the X-ray diffraction spectrum (adopting x-ray diffractometer XRD-600) of two kinds of different enamel, wherein, A is the spectral line of rare earth doped oxide compound according to the abovementioned embodiments of the present invention and nano silicon enamel coating material, and B is the spectral line of the enamel coating material of prior art.Improve SiO in enamel adding of nano silicon as can see from Figure 4
2content, improves the integrity of silicate network structure, is conducive to the raising of enamel coating acid-resistant chemical stability.Adding of rare earth oxide, in enamel coating, there is not rare earth-boron silicate compound, it can thus be appreciated that rare earth oxide the chemical reaction destroying silicate network complete structure does not occur with enamel, detrimentally affect be there is no to enamel chemical stability.
Claims (10)
1. a preparation method for industrial enamel matrix material, the method comprises to grind the mixture that the mode added introduces a certain proportion of nano silicon and rare earth oxide simultaneously in vitreous enamel, and comprises the following steps:
A) weighing step, raw materials weighing, mixes;
B) drying step, is placed in loft drier dry 1.5 hours by the raw material mixed, to remove moisture in raw material and gas;
C) high temperature melting step, puts into crucible by raw material complete for drying, is at high temperature incubated, until wire drawing is without node;
D) quenching Step, is quickly cooled to room temperature by the raw material after fusing, obtain quenching broken after frit, then dry;
E) ball milling pulping stage, is broken into powder by dried frit ball milling powder, and the mixture weighing rare earth oxide and nanometer grade silica adds additive as mill, is milled to 200 orders after mixing.
2. method according to claim 1, the ratio of mixture that wherein said powder and mill add additive is:
Powder: 90 ~ 96%,
Rare earth oxide: 3 ~ 6%,
Nano silicon: 1 ~ 4%.
3. method according to claim 1, is characterized in that
Described rare earth oxide is at least one selected from cerium oxide or lanthanum trioxide.
4. method according to claim 1, is characterized in that comprising further:
F) airtight ageing 24 hours after adding appropriate alcohol.
5., according to the method for one of claim 1-4, it is characterized in that comprising further:
G) spraying process, uniformly sprays with spray gun on steel plate by glaze slip;
H) fire step, dried steel plate is at high temperature fired.
6., according to the method for one of claim 1-4, it is characterized in that
Described step B) comprising: the raw material mixed is put into 750 DEG C of loft drier dry 1.5 hours.
7. method according to claim 6, is characterized in that
The material of described raw material consists of: zinc oxide 7%, silicon-dioxide 42.5%, aluminum oxide 5.7%, titanium oxide 2%, nickel oxide 2.5%, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 3.9%, Vanadium Pentoxide in FLAKES 2.4%, Calcium Fluoride (Fluorspan) 3.9%, boric acid 33.7%, sodium carbonate 27.4%;
Described step C) comprising: raw material complete for drying is put into crucible, at 1200 ~ 1300 DEG C, is incubated 1.5 hours, until wire drawing is without node,
Described step D) comprising: drop into immediately in cold water after the raw material after fusing is taken out.
8., according to the method for one of claim 1-4, it is characterized in that
Described step e) comprising: the mixture adding 3% cerium dioxide and 1% silicon-dioxide in the powder of frit ball mill pulverizing after the drying, the ratio being 25:1 in ball material weight ratio adds corundum abrading-ball in ball grinder, grinds 24 hours, crosses 200 mesh sieves.
9. method according to claim 5, is characterized in that
Described step G) comprising: after glaze slip being uniformly sprayed on steel plate with spray gun, drying 1.5 hours at 100 DEG C;
Described step H) comprise and dried steel plate is put in retort furnace, at 930 DEG C, fire 5-7 minute.
10. with the industrial enamel matrix material prepared according to the method for one of claim 1-9.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106119848A (en) * | 2016-07-10 | 2016-11-16 | 上海大学 | The nanometer enamel of surface of low-carbon steel is combined preparation method and the hot rolling process thereof of the sintering enamelled coating of slip |
| CN106430966A (en) * | 2016-08-18 | 2017-02-22 | 佛山欧神诺陶瓷股份有限公司 | Transparent glaze with anti-electrostatic function and preparation method for ceramic tiles of transparent glaze |
| CN106521398A (en) * | 2016-07-10 | 2017-03-22 | 上海大学 | Method for spraying enamel coating on titanium alloy surface through plasma technique and hot rolling treatment |
| CN106977101A (en) * | 2017-05-04 | 2017-07-25 | 钦州学院 | Frit for porcelain enamel with higher hardness |
| CN106977100A (en) * | 2017-05-04 | 2017-07-25 | 钦州学院 | The good frit for porcelain enamel with steel plate adherence |
| CN108863080A (en) * | 2018-08-10 | 2018-11-23 | 江西正强电瓷电器有限公司 | The preparation method of the porcelain insulator glaze of positive temperature coefficient |
| CN109052950A (en) * | 2018-09-30 | 2018-12-21 | 李文文 | A kind of pottery sky blue glaze and preparation method thereof |
| CN110255909A (en) * | 2019-07-02 | 2019-09-20 | 宁波市金象厨具有限公司 | A kind of pot body enamel coating and preparation method thereof |
| CN111116184A (en) * | 2019-12-30 | 2020-05-08 | 常州市昊天管道成套有限公司 | Oil-resistant steel pipe and manufacturing process thereof |
| CN112358185A (en) * | 2020-11-30 | 2021-02-12 | 湖南景翌湘台环保高新技术开发有限公司 | Enamel base coat and preparation method thereof |
| CN112376048A (en) * | 2020-11-30 | 2021-02-19 | 湖南景翌湘台环保高新技术开发有限公司 | Application method of enamel surface glaze grinding material |
| CN112408790A (en) * | 2020-12-04 | 2021-02-26 | 胜利新大新材料股份有限公司 | Glass-lined glaze, anti-corrosion layer in oil field pipeline and preparation method of anti-corrosion layer |
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| CN101497496A (en) * | 2008-02-02 | 2009-08-05 | 比亚迪股份有限公司 | Porcelain enamel glaze composition, film coating material and preparation thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106119848B (en) * | 2016-07-10 | 2019-04-02 | 上海大学 | The preparation method and its hot rolling treatment of the sintering enamelled coating of the compound slurry of the nanometer enamel of surface of low-carbon steel |
| CN106521398A (en) * | 2016-07-10 | 2017-03-22 | 上海大学 | Method for spraying enamel coating on titanium alloy surface through plasma technique and hot rolling treatment |
| CN106119848A (en) * | 2016-07-10 | 2016-11-16 | 上海大学 | The nanometer enamel of surface of low-carbon steel is combined preparation method and the hot rolling process thereof of the sintering enamelled coating of slip |
| CN106430966A (en) * | 2016-08-18 | 2017-02-22 | 佛山欧神诺陶瓷股份有限公司 | Transparent glaze with anti-electrostatic function and preparation method for ceramic tiles of transparent glaze |
| CN106430966B (en) * | 2016-08-18 | 2019-04-12 | 佛山欧神诺陶瓷有限公司 | A kind of preparation method of clear frit and its ceramic tile with anti-static function |
| CN106977100A (en) * | 2017-05-04 | 2017-07-25 | 钦州学院 | The good frit for porcelain enamel with steel plate adherence |
| CN106977101A (en) * | 2017-05-04 | 2017-07-25 | 钦州学院 | Frit for porcelain enamel with higher hardness |
| CN108863080A (en) * | 2018-08-10 | 2018-11-23 | 江西正强电瓷电器有限公司 | The preparation method of the porcelain insulator glaze of positive temperature coefficient |
| CN108863080B (en) * | 2018-08-10 | 2021-04-16 | 江西正强电瓷电器有限公司 | Preparation method of porcelain insulator glaze with positive temperature coefficient |
| CN109052950A (en) * | 2018-09-30 | 2018-12-21 | 李文文 | A kind of pottery sky blue glaze and preparation method thereof |
| CN110255909A (en) * | 2019-07-02 | 2019-09-20 | 宁波市金象厨具有限公司 | A kind of pot body enamel coating and preparation method thereof |
| CN110255909B (en) * | 2019-07-02 | 2022-04-01 | 宁波市金象厨具有限公司 | Enamel coating for pot body and preparation method thereof |
| CN111116184A (en) * | 2019-12-30 | 2020-05-08 | 常州市昊天管道成套有限公司 | Oil-resistant steel pipe and manufacturing process thereof |
| CN112358185A (en) * | 2020-11-30 | 2021-02-12 | 湖南景翌湘台环保高新技术开发有限公司 | Enamel base coat and preparation method thereof |
| CN112376048A (en) * | 2020-11-30 | 2021-02-19 | 湖南景翌湘台环保高新技术开发有限公司 | Application method of enamel surface glaze grinding material |
| CN112358185B (en) * | 2020-11-30 | 2023-06-09 | 湖南景翌湘台环保高新技术开发有限公司 | Enamel primer and preparation method thereof |
| CN112408790A (en) * | 2020-12-04 | 2021-02-26 | 胜利新大新材料股份有限公司 | Glass-lined glaze, anti-corrosion layer in oil field pipeline and preparation method of anti-corrosion layer |
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Application publication date: 20160127 |