CN1259588A - Method of forming ceramic coating on metal surface by utilizing laser assisted self spreading - Google Patents
Method of forming ceramic coating on metal surface by utilizing laser assisted self spreading Download PDFInfo
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Abstract
The present invention relates to method of forming ceramic coating on metal surface using laser assisted self extending which is characterized in that: take two or more than two reactant powder which can proceed SHS reaction, formulate according to stoichiometry, add in 0-40% additive mixevenly, then coat on metal surface; under the assisted action of laser with energy density 1.5X100-5.0x100 J/sq.cm. to produce self extending reaction and form ceramic coating. Advantages: (1) form ceramic coating with transition layer directly on metal surface, reduces raw material cost, (2). save energy, (3) easy to control.
Description
The invention relates to preparation of a ceramic coating on a metal surface, belonging to the field of material surface engineering. The ceramic coating is coated on the metal surface, so that the wear resistance, corrosion resistance or high temperature resistance of the material can be improved. There are many methods for forming ceramic coatings on metal surfaces, and laser sintering is one of the most used methods. Ninety is a Chinese medicinal compositionThe research of coating ceramic coating on the metal surface by using the laser sintering method in the early years is greatly developed, and people widely research Al2O3、SiO2TiC and ZrO2And the like, in the case where the unit system or the multi-component system forms a ceramic on the surface of the metal. But due to the reflection of the laser by the metal, in particular the CO by the metal surface2The laser with the wavelength of 10.6 mu m emitted by the laser has poor absorption capacity, so that the thermal efficiency of laser heating is small. At present, under the laser power lower than 2000W, a single laser surface coating technology can only form a melting mixed layer of ceramics and metal, and a complete and continuous ceramic coating cannot be prepared on the surface of the metal. Good ceramic coating can be formed only at laser power of 5000-10000W or more, however, too high laser power causes the following problems: 1) complicated equipment and high cost, and 2) the process is not easy to control and has the phenomena of burning loss and serious sputtering.
Self-propagating High-temperature synthesis (hereinafter abbreviated as SHS) technology is originated from the former Soviet Union and is mainly used for preparing TiB2The development of TiC and other pure ceramic powder can prepare hundreds of pure ceramic powder and various ceramic composite materials at present after twenty years of development, but the application of the SHS technology in the aspect of metal surface engineering is not deeply and widely researched, and particularly, the ceramic coating directly formed on the metal surface has the following two problems that 1) when the metal surface is not preheated or the preheating temperature is below 500 ℃, the single SHS method can not form the ceramic coating by carrying out the SHS reaction on the metal surface, although the adiabatic temperature of a plurality of SHS reactions can reach 2000-3000 ℃, because the metal has good thermal conductivity and the SHS reaction layer is thinner, the total heat release is less, the metal surface cannot be in a molten state by the SHS reaction on the metal surface in a short time, and the generated ceramic component can not be fused with the metal, so the method for forming the ceramic coating on the metal surface by using the single SHS method coating process is infeasible, 2) when the preheating temperature of the metal surface is more than 500 ℃, the metal surface can be melted and formed into ceramic at a certain temperature according to different SHS reaction heat release amountsThe coating, however, preheating the metal substrate to a higher temperature causes deformation and in subsequent cooling, the ceramic layer is liable to peel off due to thermal stress caused by mismatch of thermal expansion of the metal and the ceramic, and in addition, heating the workpiece to 500 ℃ or more while laser scanning is difficult and there is little operability for a large workpiece.
The invention aims to overcome the defect that the surface coating technology of the prior art can not prepare a complete continuous ceramic coating on the metal surface under low laser power and can not prepare a complete continuous ceramiccoating under high laser powerThe ceramic coating is formed, the equipment is complex, the cost is high, the process is not easy to control, and the defects of burning loss and sputtering are overcome; simultaneously overcomes the defects that the ceramic coating can not be formed on the metal surface at the low temperature of the SHS reaction and the operability is poor when the ceramic coating is formed on the metal surface at the high temperature, and aims to directly prepare the complete and continuous Al with the metal transition layer and strong bonding with the metal matrix on the metal surface2O3、TiB2、TiC、SiO2And ZrO2Ceramic coating, the technical solution of the invention is provided.
The basic idea of the invention is that, according to the principle that the SHS reaction is a high exothermic chemical reaction process, the SHS technology is combined with the laser technology, a layer of powder and additive powder which can generate ceramic coating by SHS reaction is coated on the metal surface, the coating is ignited by laser and self-propagating reaction is generated, because the chemical reaction process is continuously carried out under the support of high heat released by the laser and the coating, under the premise of keeping the melting of the ceramic powder and the additive and the melting of the metal surface at the same time of reaction, the SHS reaction is propagated to the whole metal surface, the generated ceramic component is fully fused with the molten metal surface, the metal in the material is melted and a metal transition layer is formed between the metal substrate and the ceramic coating, thereby forming a complete and continuous ceramic coating and realizing the task of the invention.
The invention provides a method for forming a ceramic coating on a metal surface by utilizing laser-assisted self-propagating, which is characterized by comprising the following steps: two or more than two are taken according to the stoichiometric proportionReactant powder for SHS reaction and metal powder Cr, Mo, W, Zr or ceramic powder Al accounting for 0-40% of the total weight of the reactants2O3、ZrO2、SiO2The like or the mixture of the like is used as additive powder, and the powder is uniformly mixed for 5 to 20 minutes and then coated on the surface of the metal; with an energy density of 1.5X 103～5.0×103J/cm2The laser is scanned on the coating layer of the metal surface, at the moment, the coating layer is ignited and generates self-propagating reaction, under the condition that the laser scanning and the self-propagating reaction are carried out simultaneously, the surface layer of the metal matrix is melted under the action of a large amount of heat released by the self-propagating reaction and laser heating, the molten or liquid self-propagating reaction product is fused with the metal surface, and an Al intermediate transition layer with metal is formed on the metal surface2O3、TiB2、TiC、SiO2And ZrO2The formula for calculating the laser energy density of (1) is P/(V.D), wherein P is the laser power (in W), V is the scanning speed (in mm/s), and D is the laser spot diameter (in mm). It is further characterized in that: in order to obtain the metal intermediate transition layer, the adopted method is that when the reaction material adopts powder which can carry out self-propagating reaction and generate ceramic material and metal material or adopts reaction powder which can carry out self-propagating reaction but only can generate ceramic material but not can generate metal material, metal material additives are additionally added into the reactant powder, and the ceramic coating with the metal intermediate transition layer can be obtained after laser and self-propagating reaction: the process steps of the inventionare as follows:
first step of proportioning
According to the weight ratio requirement of the formula of the invention, reactant powder capable of performing SHS reaction and metal powder Cr, Mo, W, Zr and the like or ceramic powder Al accounting for a certain weight of the reactants are taken2O3、ZrO2、SiO2Or the like or the mixture of the components as additive powder for blending,
second step mixing
Uniformly mixing the prepared powder for 5-20 minutes to obtain a material,
third step of coating
And coating the mixed material on the polished metal surface, wherein the specific coating method has two conditions:
1) adopting wet coating, namely adding a proper amount of water or aqueous solution of carboxymethyl cellulose into powder, uniformly stirring, spraying or manually brushing on the surface of a ground workpiece,
2) dry coating is adopted, namely a powder feeding device is used for spraying the mixed material to a laser scanning area on the surface of a workpiece, and SHS reaction and laser sintering are carried out simultaneously,
the fourth step is drying
When dry coating is adopted, drying is not needed, and when wet coating is adopted, drying is carried out for 1-2 hours at 110-120 ℃ after coating to remove water in the coating,
fifth step laser-assisted sintering
The process adopts energy density of 1.5 × 103～5.0×103J/cm2The laser is scanned on the metal surface to heat and ignite the workpiece coating, the metal surface coating generates self-propagating reaction to form a ceramic coating with a metal intermediate transition layer,
the sixth step is to stop the machine and check the quality
And (5) inspecting the thickness and the surface quality of the ceramic layer and the intermediate transition layer of the workpiece, and using the workpiece after the ceramic layer and the intermediate transition layer are qualified.
The invention can form a metal intermediate transition layer between a metal matrix and a ceramic coating, and the forming process comprises the following steps: the metal generated by the self-propagating reaction or the metal in the additive is melted under the action of self-propagating heat release and laser, and because the specific gravity of the molten metal and the affinity of the molten metal and the surface of the metal substrate are both greater than those of the molten ceramic, a metal transition layer is formed between the metal substrate and the ceramic coating, the internal stress of the ceramic material coating is reduced, and the bonding strength is improved; the main component of the ceramic coating on the metal surface is TiB2、TiC、Al2O3And ZrO2They are not formed by ceramic powders directly coated on the metal surface under laser sintering, but are products synthesized by self-propagating reactions.
The self-propagating reaction for forming the ceramic coating is mainly a reaction represented by the following reaction formula or a reaction obtained by mixing the following reaction formulae in different proportions:
in the formula, Tad is the highest temperature reached by the system, namely the adiabatic temperature, which is ignited for reaction at 25 ℃ (298K) under the adiabatic condition without heat loss; the conditions of adding 0 or 40 percent of additives in the invention mean that: when there is metal in the self-propagating reaction product, such as: reaction formula (C) or (D), optionally without addition of additives; other cases, such as: the reaction formula (A) or (B) is shown, and the highest addition amount is 40 percent; the laser energy density range adopted by the invention is 1.5 multiplied by 103～5.0×103J/cm2When the heat release of the SHS reaction is large and a small amount of the additive is added or the additive is not added, the laser energy density takes a lower limit, and when the heat release of the SHS reaction is small and a large amount of the additive is added, the laser energy density takes an upper limit.
The main advantages of the invention are: 1) directly forming a ceramic coating with a transition layer on the metal surface, overcoming the defects of a single laser method and a single self-propagating method, reducing the cost of raw materials, 2) the ceramic coating is directly generated by reactants under the auxiliary action of laser by an SHS reaction, saving the cost of materials, 3) saving energy, reducing the cost of equipment, and the energy density of the laser in actual operation is 1.5 multiplied by 103～5.0×103J/cm2Generally, the metal surface can be formed to form a ceramic coating with the laser power below 1000W, which is 1/5-1/3 of the power of the ceramic coating prepared with high laser power, saves energy by more than 2-3 times, and is easy to control and small in burning loss and sputtering phenomena.
The details of the present invention are further described below in conjunction with the specific embodiments of the present invention.
Example 1
On a 45 steel wear-resistant block with the thickness of 6mm and the thickness of 30 multiplied by 50mm, the surface is required to be coated with a layer of Al with the thickness of 0.2mm2O3+TiB2The ceramic coating is prepared by the method with the metal intermediate transition layer being Cr, and the method comprises the following steps:
first step of proportioning
The coating material consists of Al2O3 and TiB2, according to the SHS reaction equation: respectively taking 6.48g of Al powder with the granularity of 200-270 meshes and TiO powder25.76g of powder, B2O35.04g of powder, 3.46g of Cr (wt%, same below) based on 20% of the total amount of the above reactants as an additive, and 20.7 g of the total weight.
Second step ball milling and mixing
Directly putting the powder into a ball mill for dry mixing for 20 minutes to prepare the required material,
third step of workpiece polishing
And (5) pickling the surface of the workpiece to remove dirt, and polishing the workpiece to be smooth to 200# abrasive paper.
Fourth step of material coating
Adding 10ml of water into the materials, uniformly stirring, manually brushing the materials on the surface of a workpiece with the thickness of 0.5mm, and drying the workpiece at the temperatureof 115-120 ℃ for 2h to remove water.
Fifth step laser-assisted sintering
Taking the laser energy density at 2.5 multiplied by 103J/cm2At the moment, the laser power is 500W, the scanning speed is 5mm/s, the spot diameter is 4mm, the laser is enabled to continuously scan the metal surface, the spot overlap joint is 0.5mm each time, the coating layer is ignited under the laser heating for self-propagating reaction, the surface layer melting occurs under the action of the self-propagating reaction releasing large amount of heat and the laser heating, and the self-propagating reaction product Al is generated2O3+TiB2Molten or liquid under self-heat release and laser heating conditionsThe surface is fused to form a continuous ceramic material coating, and meanwhile, the additive Cr forms a metal intermediate transition layer between the metal matrix and the ceramic coating, so that the bonding strength is improved.
The sixth step is to stop and check
The surface of the ceramic coating prepared by detection is smooth, complete and continuous, and the surface coating is Al2O3+TiB2The thickness of the layer is 0.15mm, and the thickness of the middle transition layer Cr is 0.05 mm.
Examples 2, 3, 4, 5 below, which are similar to example 1 in preparation steps and procedure, and therefore similar steps are omitted, can be seen in example 1, and only workpiece or sample dimensions, ceramic coating requirements, dosing and laser processing parameters are given for the examples below.
Example 2
On a 40Cr axis of phi 50X 800mm, the workpiece requires a layer of 0.25mm ZrO2+Al2O3The ceramic coating is prepared by the method, wherein the intermediate transition layer is Cr,and the method comprises the following process parameters:
the SHS reaction equation is: adding 40% of Al2O3And (3) wet coating, adding a proper amount of 0.5% carboxymethyl cellulose aqueous solution, uniformly stirring, manually brushing a coating with a thickness of 0.6mm on the surface of the workpiece, and drying the workpiece at the temperature of 115-120 ℃ for 2h to remove water. The laser energy density was 4.0X 103J/cm2At the moment, the laser power is 800W, the scanning speed is 5mm/s, the spot diameter is 4mm, the ceramic coating prepared by detection is complete and continuous, and ZrO is2+Al2O3The thickness of the layer is 0.15mm, and the thickness of the middle transition layer Cr is 0.1 mm.
Example 3
On a 40X 60mm, 10 thick corrosion resistant block of 18-8 stainless steel, a 0.2mm thick layer of Al is required2O3The TiC ceramic coating is prepared by adopting the method, wherein the middle transition layer is W, and the technological parameters are as follows:
the SHS reaction equation is: the additive is W accounting for 40% of the total reactant, and the laser energy density is 5.0 × 103J/cm2In this case, the laser power was 1000W, the scanning speed was 5mm/s, and the spot diameter was 4 mm.
Example 4
On cast iron specimens 50X 80mm, 12mm thick, a layer of 0.25mm ZrO was prepared2+Al2O3+SiO2The ceramic coating is prepared by the method, wherein the intermediate transition layer is Cr, and the method comprises the following process parameters:
the SHS reaction equation is: the additive is SiO2ZrO accounting for 15 percent of the total amount of reactants25% of the total amount of reactants, and the laser energy rate density is 3.5 × 103J/cm2At this time, the laser power was 700W, the scanning speed was 5mm/s, and the spot diameter was 4 mm.
Example 5
A layer of 0.2mm Al was prepared on a 30X 50mm, 6mm thick specimen of A3 steel2O3+SiO2The ceramic coating is prepared by the method, wherein the transition layer is Cr, and the method comprises the following process parameters:
the SHS reaction equation is: the additive is SiO2Accounting for 30% of the total amount of reactants, and the laser energy rate density is 2.5 × 103J/cm2In this case, the laser power was 500W, the scanning speed was 5mm/s, and the spot diameter was 4 mm.
Claims (3)
1. The method for forming the ceramic coating on the metal surface by utilizing laser-assisted self-propagating is characterized by comprising the following steps of:
a) taking two or more than two reactant powders capable of carrying out self-propagating high-temperature synthesis reaction and metal powder or ceramic powder or a mixture of the metal powder and the ceramic powder accounting for 0-40% of the total weight of the reactants as additive powder according to the stoichiometric proportion, uniformly mixing the powder for 5-20 minutes to form a material, then coating the material on the surface of metal,
b) with an energy density of 1.5X 103～5.0×103J/cm2The laser is scanned on the coating layer of the metal surface, the coating layer is ignited and generates a self-propagating reaction, and under the condition that the laser scanning and the self-propagating reaction are carried out simultaneously, a ceramic coating with a metal transition layer is formed on the metal surface.
2. The method for forming a ceramic coating on a metal surface using laser-assisted self-propagating according to claim 1, wherein: the condition for obtaining the metal intermediate transition layer is that the reactant powder should adopt powder which can carry out self-propagating reaction and generate ceramic material and metal material or metal powder additive should be added when the reactant powder adopts the reactant powder which can carry out self-propagating reaction but only can generate ceramic material but can not generate metal material.
3. The method for forming ceramic coating on metal surface by laser-assisted self-propagating according to claim 1 or 2, wherein the process steps are characterized in that:
first step of proportioning
The powder is prepared according to the weight ratio of the formula of the invention,
second step mixing
The prepared powder is mixed into a uniform material,
third step of coating
The evenly mixed material is coated on the surface of the polished workpiece by a wet method or a dry method, wherein the wet method is to add water or a carboxymethyl cellulose aqueous solution into the mixed material to be evenly stirred and then to be coated on the surface of the polished workpiece, the dry method is to synchronously spray the material on the surface of the polished workpiece in a laser scanning area while scanning the laser,
the fourth step is drying
When dry coating is adopted, drying is not needed, when wet coating is adopted, drying is carried out for 1-2 h at 110-120 ℃ after coating,
fifth step laser-assisted sintering
By adopting the laser parameters of the invention, the workpiece coating is heated and ignited, the metal surface coating generates self-propagating reaction to generate a ceramic coating with a metal intermediate transition layer,
and step six, stopping the machine and checking the quality.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 98123920 CN1131895C (en) | 1998-11-03 | 1998-11-03 | Method of forming ceramic coating on metal surface by utilizing laser assisted self spreading |
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| CN 98123920 CN1131895C (en) | 1998-11-03 | 1998-11-03 | Method of forming ceramic coating on metal surface by utilizing laser assisted self spreading |
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| CN1131895C CN1131895C (en) | 2003-12-24 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102689096A (en) * | 2012-06-07 | 2012-09-26 | 哈尔滨工业大学 | Method for laser-induced self-propagating connection between carbon fiber reinforced aluminum-based composite and metal |
| CN105237791A (en) * | 2015-10-14 | 2016-01-13 | 哈尔滨工业大学 | Method for preparing cladding coating on surface of carbon fiber reinforced thermo plastic by laser-assisted self-propagation high-temperature synthesis (SHS) technology |
| CN105458269A (en) * | 2015-12-01 | 2016-04-06 | 南通大学 | Manufacturing method of wear-proof coating |
| CN108723363A (en) * | 2017-04-14 | 2018-11-02 | 中南大学 | It is a kind of ceramics and/or refractory metal between compound increase material manufacturing method |
| CN109760173A (en) * | 2019-03-07 | 2019-05-17 | 西北工业大学 | Wall-like Al2O3-GdAlO3-ZrO2The laser of ternary eutectic ceramics melts manufacturing process |
| CN110256092A (en) * | 2019-07-30 | 2019-09-20 | 华东师范大学重庆研究院 | A kind of heat barrier coat material and preparation method thereof |
| CN111095499A (en) * | 2018-05-15 | 2020-05-01 | 东京毅力科创株式会社 | Method for forming member and plasma processing apparatus |
-
1998
- 1998-11-03 CN CN 98123920 patent/CN1131895C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102689096A (en) * | 2012-06-07 | 2012-09-26 | 哈尔滨工业大学 | Method for laser-induced self-propagating connection between carbon fiber reinforced aluminum-based composite and metal |
| CN105237791A (en) * | 2015-10-14 | 2016-01-13 | 哈尔滨工业大学 | Method for preparing cladding coating on surface of carbon fiber reinforced thermo plastic by laser-assisted self-propagation high-temperature synthesis (SHS) technology |
| CN105237791B (en) * | 2015-10-14 | 2018-07-03 | 哈尔滨工业大学 | A kind of method for preparing cladding coating on fibre reinforced thermoplastic composite surface using laser assisted SHS techniques |
| CN105458269A (en) * | 2015-12-01 | 2016-04-06 | 南通大学 | Manufacturing method of wear-proof coating |
| CN108723363A (en) * | 2017-04-14 | 2018-11-02 | 中南大学 | It is a kind of ceramics and/or refractory metal between compound increase material manufacturing method |
| CN111095499A (en) * | 2018-05-15 | 2020-05-01 | 东京毅力科创株式会社 | Method for forming member and plasma processing apparatus |
| CN109760173A (en) * | 2019-03-07 | 2019-05-17 | 西北工业大学 | Wall-like Al2O3-GdAlO3-ZrO2The laser of ternary eutectic ceramics melts manufacturing process |
| CN109760173B (en) * | 2019-03-07 | 2020-11-20 | 西北工业大学 | Wall-like Al2O3-GdAlO3-ZrO2Laser melting forming method of ternary eutectic ceramics |
| CN110256092A (en) * | 2019-07-30 | 2019-09-20 | 华东师范大学重庆研究院 | A kind of heat barrier coat material and preparation method thereof |
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