CN101787478B - Mixing method of titanium carbonitride base metal ceramic using water as medium - Google Patents
Mixing method of titanium carbonitride base metal ceramic using water as medium Download PDFInfo
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Abstract
A mixing method of titanium carbonitride base metal ceramic using water as medium uses water to replace commonly used absolute ethyl alcohol as the mixing medium and completes the mixing process of metal ceramic powder by adding polyethyleneimine as dispersing agent to assist the adjustment of pH value. By adopting water as the mixing medium for preparing Ti(C,N) base metal ceramic, the energy can be effectively saved and the production cost is lowered. The polyethyleneimine is a water-soluble polymer which can be well dissolved in the slurry using water as the mixing medium. As the dispersing agent, the polyethyleneimine mainly uses the adsorption on a solid-liquid interface to form an adsorption layer for preventing the mutual contact between particles, thereby improving the dispersibility of the system and leading a microstructure of a sintered body to be fine and uniform. In the compacting process, the polyethyleneimine wraps on the surface of the powder particle and works as lubricant and molding agent, thereby improving the uneven distribution of the green density, reducing the deformation of the sintered body and improving the mechanical property of the sintered body.
Description
Technical field
The invention belongs to the base titanium carbonitride preparation field, be specifically related to a kind of titanium carbonitride based cermet mixed material method.
Background technology
Batch mixing is the essential operation of sintering metal preparation process, its objective is for each component powders is mixed.(C N) adopts material by wet type mixing in the based ceramic metal preparation process, adds dehydrated alcohol, acetone and other organic solvent liquid medium in the batch mixing process at Ti.Requirement to the batch mixing medium is: not with powder generation chemical reaction, and nontoxicity, wide material sources and with low cost, lower boiling is volatile etc.At present, prepare the WC-Co Wimet with alternative dehydrated alcohol of water or acetone as the batch mixing medium and obtained Preliminary Applications.And Ti (C, N) based ceramic metal is owing to complicated component, and each component powders hydrolysising property is different, and Shang Weijian is with the report of water as the batch mixing media applications.
In addition, (particle diameter of raw materials used powder is more and more littler for C, N) based ceramic metal in order to obtain close grain Ti.Because powder diameter reduces to have increased its surface energy, reunites easily between the powder particle.In case the formation coacervate will bring detrimentally affect to compression moulding, sintering process, thereby cause product performance to descend.Therefore, (C, N) based ceramic metal must overcome the agglomeration traits of powder particle to obtain high performance Ti.At present, one of effective way that overcomes reunion is that powder is dispersed in the medium, by pH, the adding dispersion agent of regulation system, and imposes ultrasonic wave or other mechanical means, and it is disperseed at the dispersion medium camber.
Summary of the invention
The objective of the invention is to provide to add the dehydrated alcohol that a kind of water consumption substitution generally uses at present and be the batch mixing medium, by adding polymine, and carry out the method for titanium carbonitride based cermet mixed material by technological measures such as adjusting pH values as dispersion agent.
The object of the present invention is achieved like this: a kind of is the method for mixing of the base titanium carbonitride of medium with water, and take by weighing and insert in ball grinder by following weight percent powder stock: TiC 20～40; TiN 5～15; Mo 0～17; WC 0～20; Ni 20～36; C 1.0～2.2, add sintered carbide ball and water after, add 0.1～1.0% polyethylene of dispersing agent imines of powder stock quality again, regulate slip pH value between 9～11, on ball mill, carry out ball mill mixing, gained slip behind the ball milling is finished the batch mixing operation.The sintered carbide ball add-on is 4～8: 1 with the mass ratio of the raw material that is added, and drum's speed of rotation is 150～250 rev/mins, and the ball milling time is 24～48 hours.The add-on of water is just to have flooded sintered carbide ball and raw material.What be used to regulate slip pH value is ammoniacal liquor.
Titanium carbonitride based cermet mixed material method provided by the invention, (effectively save energy reduces manufacturing cost for C, N) based ceramic metal for the batch mixing medium prepares Ti to adopt water.Polymine (PEI) is a water-soluble polymers, can water-solublely well be in the slip of batch mixing medium.As dispersion agent, polymine (PEI) mainly is to utilize its adsorption on solid-liquid interface, forms an adsorption layer and hinders intergranular being in contact with one another, and improves the dispersiveness of system, makes the microstructure of sintered compact tiny, even; In pressing process, PEI is coated on powder particle surface, has played the effect of lubricant and forming agent, improves the ununiformity that pressed density distributes, and alleviates the sintered compact distortion, improves Ti (C, N) mechanical property of based ceramic metal of preparation.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is Ti (C, N) the sedimentation photo of based ceramic metal mixed powder.
Fig. 2 is Ti (C, N) subsidence curve of based ceramic metal mixed powder.
Fig. 3 adds PEI and does not add the Ti of PEI preparation that (left side is the sample of interpolation PEI for C, N) the sintering warpage situation of based ceramic metal; The right side is not for adding the sample of PEI.
Fig. 4 is Ti (C, N) microstructure picture of the scanning electronic microscope back scattering mode imaging of based ceramic metal of adding PEI and not adding the PEI preparation.
Fig. 5 is Ti (C, N) microstructure picture of the scanning electronic microscope back scattering mode imaging of based ceramic metal of not adding the PEI preparation.
Embodiment
Example 1: according to table 1 preparation 10g sintering metal mixed powder, add 20mL water, add the polymine (PEI) of the 0.386wt% of powder stock again, regulate pH to 10.25 with ammoniacal liquor.The slip that configures is put into the ultrasonic wave biochemical instruments 20min that vibrates, pour into rapidly then in the 25ml graduated cylinder, carry out sedimentation observation.Evaluate dispersed quality qualitatively by the sedimentation situation of observing slip, sedimentation phenomenon is not obvious, and dispersiveness is good more, and slip is stable; Otherwise, slip instability then.
Table 1Ti (C, N) content of each component powders of based ceramic metal and particle diameter
Fig. 1 is after placing 26h, adds PEI and does not add Ti (C, N) the sedimentation photo of based ceramic metal mixed powder in water of PEI.As can be seen from the figure, PEI can improve the dispersiveness of slip significantly.After having added the slip placement 26h of PEI, overall appearance still shows as the outstanding turbid body of aterrimus, good dispersity; Tangible sedimentation has taken place in the slip that does not add PEI, and outward appearance shows as transparent liquid, bad dispersibility.
Fig. 2 is Ti (C, N) the settling volume curve of based ceramic metal mixed powder in water that adds PEI and do not add PEI.It is fast and sinkability is big not add the slip sedimentation of PEI, and the slip sedimentation of adding PEI is slow, and sinkability is little, illustrates that PEI has effectively improved the dispersion stabilization of slip.
Example 2: example 1 batch mixing condition is used for Ti (C, N) preparation of based ceramic metal.Preparation process is as follows:
According to table 1 preparation total amount is that the sintering metal mixed powder of 2Kg carries out ball milling, is ball-milling medium with water, adds the 0.335wt% polymine (PEI) of mixed powder, regulate pH to 10.31 with ammoniacal liquor, ratio of grinding media to material is 5: 1, and rotating speed is 200r/min, ball milling time 36h.Slip drying behind the ball milling, grind after, compression moulding under the pressing force of 200MPa is with after degreasing, sinter Ti (C, N) based ceramic metal into.
Table 2 is to add PEI and do not add the measured pressed density of PEI batch mixing powder.The density of adding PEI formation pressed compact under example 1 and example 2 batch mixing conditions has increased about 3.2%.As seen PEI helps compression moulding.
Table 2Ti (C, N) density of based ceramic metal sample base
(interpolation PEI can effectively reduce the sintering warpage of sample to Fig. 3 for C, N) the sintering warpage situation of based ceramic metal in order to add PEI and not add the Ti of PEI preparation.
Table 3 has been listed Ti (C, N) bending strength of based ceramic metal of adding dispersion agent PEI and not adding dispersion agent PEI preparation.The mensuration of bending strength is followed GB 3851-83.After adding PEI, the powder dispersiveness obtains bigger improvement, and pressed density improves, and its bending strength of the sample that sintering goes out is apparently higher than the sample that does not add PEI, and amplification is about 19.2%.
Table 3Ti (C, N) bending strength of based ceramic metal
Fig. 4 and Fig. 5 are respectively the microstructure picture of adding PEI and not adding the scanning electronic microscope back scattering mode imaging of PEI (b) sample.Record with division lines method: add the PEI preparation Ti (C, N) based Cermet hard phase average grain-size is 1.07 μ m, (C, N) based Cermet hard phase average grain-size is 1.60 μ m not add the Ti of PEI preparation.(C, N) tissue of based ceramic metal is than the sintered article homogeneous microstructure of not adding PEI, tiny for the Ti of interpolation PEI preparation.As seen PEI has improved the mixed powder dispersiveness effectively.
Claims (4)
1. one kind is the method for mixing of the base titanium carbonitride of medium with water, and it is characterized in that: take by weighing and insert in ball grinder by following weight percent powder stock: TiC 20～40; TiN 5～15; Mo 0～17; WC 0～20; Ni 20～36; C 1.0～2.2, add sintered carbide ball and water after, add 0.1～1.0% polyethylene of dispersing agent imines of powder stock quality again, regulate slip pH value between 9～11, on ball mill, carry out ball mill mixing, gained slip behind the ball milling is finished the batch mixing operation.
2. according to claim 1 a kind of be the method for mixing of the base titanium carbonitride of medium with water, it is characterized in that: the sintered carbide ball add-on is 4～8: 1 with the mass ratio of the raw material that is added, drum's speed of rotation is 150～250 rev/mins, and the ball milling time is 24～48 hours.
3. according to claim 1 a kind of be the method for mixing of the base titanium carbonitride of medium with water, it is characterized in that: the add-on of water is just to have flooded sintered carbide ball and raw material.
4. according to claim 1 a kind of be the method for mixing of the base titanium carbonitride of medium with water, it is characterized in that: what be used to regulate slip pH value is ammoniacal liquor.
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