Dispersants for slurries with lithium iron phosphate
By incorporating a specific dispersant and alkanolamine into the lithium iron phosphate slurry, the viscosity is managed to allow for higher solid content, addressing the challenge of maintaining efficient spray drying and improving production efficiency.
Patent Information
- Application Number
- PCT/CN2023/126642
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2023-10-26
- Publication Date
- 2025-05-01
AI Technical Summary
The challenge in lithium iron phosphate (LFP) production is to increase the solid content of the slurry while maintaining a viscosity below 400 centipoise (cP) to facilitate efficient spray drying and reduce production costs.
A lithium iron phosphate slurry is formulated using a dispersant of specific chemical structure and an alkanolamine, which are combined with iron phosphate, lithium carbonate, and water to achieve a solid content greater than 50 weight percent and a viscosity of about 200 to 700 centipoise.
The use of the dispersant and alkanolamine combination effectively reduces the viscosity of the LFP slurry, allowing for increased solid content without compromising the spray drying process, thereby enhancing production efficiency and product quality.
Smart Images

Figure CN2023126642_01052025_PF_FP_ABST
Abstract
Description
Dispersants for Slurries with Lithium Iron Phosphate
[0001] Field of Disclosure
[0002] The present disclosure relates generally to slurries and more particularly to dispersants for slurries with lithium iron phosphate.Background
[0003] Due to increasingly restrict environmental policies around the global and government's commitment towards sustainability, the electric vehicle (EV) market has been expanding rapidly for the past decade, leading to ever-growing demands for better energy storage devices. Lithium-ion battery (LiB) , the current dominating energy storage product, has therefore become one of the most popular industries.
[0004] Global EV sales continue to grow at an ever increasing rate. Battery electric vehicles (BEVs) and plug-in hybrid electric vehicles (PHEVs) will make up to >55%of new vehicle production by 2030 across China, Europe, and North America. The total global demand for the LiB market was 700 gigawatt-hours (GWh) in 2022, which is estimated to increase to 4.7 terawatt-hours (TWh) by 2030.
[0005] Among all the conventional cathode materials for LiB, lithium iron phosphate (LiFePO4, or LFP) currently dominates the market due to its low cost, high stability, and high safety performance.However, as more and more producers enter the market, competition between LFP producers has become fiercer and many key producers are looking for new ways to not only commit to their sustainability goals but also reduce their production costs.
[0006] Currently, there are three different methods for manufacturing LFP: the solid-state method, the hydrothermal method, and the sol-gel method. Among these three, the solid-state method is the most commonly used one because the process is relatively straight-forward, well-established, and relatively inexpensive to setup. A typical solid-state process involves (1) mixing all raw materials (Li source, Fe source, P source, etc. ) and disperse them in water; (2) sand-milling the mixture for 6~10 hours until the desired particle size is reached; (3) spray-drying the precursor slurry; (4) calcinating the dried mixture to get the final LFP cathode active material product.
[0007] One of the many challenges for LFP as a cathode active material is its low electronic conductivity. In order to improve battery's electrochemical performance, LFP producers have been carbon-coating LFP with varying carbon sources (such as Glucose, Lactose, Sucrose, Maltose, among other organic compounds that include carbon) to increase the electric conductivity of the active material. These carbon sources will be added together with all other solid raw materials of the process and after the calcination step of the process. The carbon sources added become a layer of residual carbon surrounding the LFP particles, which facilitates electron transport within the materials.
[0008] Another challenge faced by many LFP producers is to improve their overall production efficiency by increasing slurry solid content. Increasing the solid content can improve production efficiency and end product quality of the LFP and subsequently formed cathodes of the battery. Both sand-milling and spray-drying in the solid-state manufacturing method require either high energy input for long-time sanding milling, or high water usage for spray drying.
[0009] Currently, the most common solid content used in this industry is about 30 weight percent (wt. %) to 40 wt. %with the rest being water as the solvent. The limiting factor for any higher solid content is that when slurry viscosity reaches more than ~400 centipoise (cP) , it can become very difficult to conduct the subsequent spray drying step, as the slurry is too viscous to be sprayed to desired particle size. Thus, the solid content is not able to be increased without also increasing the viscosity and the maximum viscosity is approximately 400 cP when a spray drying step is necessary for LFP production.These shortcomings of being unable to increase the wt. %of the solid content demonstrates the continued need in the art for increasing the solid content while maintaining a viscosity that is less than a threshold for the spray drying steps.Summary
[0010] In some aspects, the techniques described herein relate to producing a lithium iron phosphate (LFP) slurry that is used as a component of a cathode slurry. Increasing the solid content of the LFP slurry results in a higher quality for the cathode slurry, however the higher solid content results in a higher viscosity which is detrimental to cathode production. The LFP slurry may have viscosity restrictions during different steps of the production. For example, the production can include a spray drying step to remove water from the LFP slurry. The spray drying step can require a viscosity that is less than 400 cP. In order to increase the solid content of the LFP slurry and maintain the viscosity below 400 cP, the present disclosure utilizes a dispersant and an alkanolamine in combination. The dispersant and alkanolamine LFP slurry addresses the shortcomings discussed herein and above.
[0011] For the present disclosure, a lithium iron phosphate (LFP) slurry, includes an iron compound, a lithium compound, a dispersant of Formula I:
[0012] where n of Formula I is an integer from 1 to 10 and R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C1 to C18 alkyl chain and R2 of Formula I is selected from a group consisting of a hydrogen, a methyl group, an ethyl group or combinations thereof, and an alkanolamine of Formula II:
[0013] where R1, R2, and R3 of Formula II is independently selected from a hydrogen or a hydroxyl alkyl group having 1 to 4 carbons.
[0014] For the present disclosure, a solid content of the iron compound and the lithium compound is greater than 50 weight percent (wt. %) of the lithium iron phosphate slurry based on the total weight of the lithium iron phosphate slurry, and the lithium iron phosphate slurry has a viscosity of about 200 to about 700 centipoise (cP) . For the present disclosure, the iron compound is iron phosphate (FePO4) and the lithium compound is lithium carbonate (Li2CO3) . For the present disclosure, the lithium iron phosphate slurry includes glucose as a carbon source. For the present disclosure, the dispersant of Formula I and the alkanolamine of Formula II are combined with the iron compound, the lithium compound and water to form an aqueous mixture.
[0015] For the present disclosure, the dispersant comprises 0.8 weight percent to 4.0 weight percent of a total weight of both the iron compound and the lithium compound. For the present disclosure, the alkanolamine is present in the slurry from 10 molar percent to 120 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. For the present disclosure, the R1 of the dispersant of Formula I is selected from the alkylphenyl group, the linear or branched group, and the primary or secondary alkyl chain group with a total of 12 to 14 carbon atoms. For the present disclosure, the molar ratio of lithium, iron, and phosphorous within the lithium iron phosphate slurry is approximately 1: 1: 1.
[0016] The present disclosure further includes a method that includes generating a lithium iron phosphate slurry including: combining an iron compound and a lithium compound, water, a carbon source with a weight percent that is greater than 40 weight percent of the lithium iron phosphate slurry, combining a dispersant of Formula I:
[0017] where n of Formula I is an integer from 1 to 10 and R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C1 to C18 alkyl chain and R2 of Formula I is selected from a group consisting of a hydrogen, a methyl group, an ethyl group or combinations thereof, and combining an alkanolamine of Formula II:
[0018] where R1, R2, and R3 of Formula II is independently selected from a hydrogen or a hydroxyl alkyl group having 1 to 4 carbons,
[0019] The method further includes performing a spray-drying process on the lithium iron phosphate slurry when a viscosity of the lithium iron phosphate slurry is less than 400 centipoise (cP) and calcinating the lithium iron phosphate mixture. For the present disclosure, the iron compound is iron phosphate (FePO4) and the lithium compound is lithium carbonate (Li2CO3) . For the present disclosure, the composition of dispersant of Formula I is within a range of 0.8 weight percent to 4.0 weight percent with respective to a total amount of active materials including the iron phosphate (FePO4) and the lithium carbonate (Li2CO3) and the composition of the alkanolamine of Formula II is within a range of 10 molar percent to 120 molar percent with respect to a molar quantity of P (OH) sites in the dispersant of Formula I.
[0020] For the present disclosure, the weight percent of the iron phosphate (FePO4) and the lithium carbonate (Li2CO3) is greater than 45 weight percent of the lithium iron phosphate slurry and the viscosity of the lithium iron phosphate slurry is less than 200 cP. For the present disclosure, the carbon source is glucose. For the present disclosure, R1 of the dispersant of Formula I is one of an octyl phenyl or nonyl phenyl.Detailed Description
[0021] In some aspects, the techniques described herein relate to producing a LFP slurry that is used as a component of a cathode slurry. Increasing the solid content of the LFP slurry results in a higher quality for the cathode slurry, however the higher solid content results in a higher viscosity which is detrimental to cathode production. The LFP slurry may have viscosity restrictions during different steps of the production. For example, the production can include a spray drying step to remove water from the LFP slurry. The spray drying step can require a viscosity that is less than 400 cP, where the viscosity is measured as described in the Examples section herein. In order to increase the solid content of the LFP slurry and maintain the viscosity below 400 cP, the present disclosure utilizes a dispersant and an alkanolamine in combination. The dispersant and alkanolamine LFP slurry addresses the shortcomings discussed herein and above.
[0022] The present disclosure describes a combined formulation of phosphoric acid ester with alkanolamine as an innovative dispersant for aqueous LFP precursor slurry. This dispersant can be added together with the other raw materials during step (1) of the solid-state process. In some examples, no additional steps are needed other than adding the dispersant with the other raw materials of the solid-state process. The general chemical structure for phosphoric acid ester is shown below as Formula I and the chemical structure for alkanolamine is shown below as Formula II. As described herein, the composition of phosphoric acid ester dispersant can range from 0.8 wt. %to 4.0 wt. %with respect to a total amount of active materials added to the LFP slurry. The active materials of the LFP slurry can include iron phosphate and / or lithium carbonate. The composition of amine can range from 10 molar percent to 120 molar percent with respect to the amount of P (OH) sites of the phosphoric acid ester dispersant.
[0023] In some examples, the phosphoric acid ester group in the dispersant has a strong affinity towards the LFP precursor slurry particles and helps to disperse the LFP particles better during a milling process. Meanwhile, alkanolamines can provide neutralization of OH groups to further stabilize the particles in water (aqueous mixture) . This dispersant formulation has demonstrated its ability to disperse particles of the LFP slurry, reduce the slurry viscosity after sand-milling, and increase the maximum solid content to greater than 50 wt. %.
[0024] For the present disclosure, a lithium iron phosphate (LFP) slurry, includes an iron compound, a lithium compound, a dispersant of Formula I:
[0025] where n of Formula I is an integer from 1 to 10 and R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C1 to C18 alkyl chain and R2 of Formula I is selected from a group consisting of a hydrogen, a methyl group, an ethyl group or combinations thereof, and an alkanolamine of Formula II:
[0026] where R1, R2, and R3 of Formula II is independently selected from a hydrogen or a hydroxyl alkyl group having 1 to 4 carbons. In a specific example, at least one of the R1, R2, and R3 of Formula II is not a hydrogen. In other examples, at least one of the R1, R2, and R3 of Formula II is hydroxyl alkyl group having 1 to 4 carbons. In another example, R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C8 to C18 alkyl chain.
[0027] In some examples, the n of Formula I is an integer from 3 to 8. In other examples, the n of Formula I is one of 5 or 7.5. In some examples, R1 of Formula I is a C10 to C16 alkylphenyl group. In a specific example, the R1 of Formula I is a C14 alkylphenyl group. In a specific example, the R2 group of Formula I is a hydrogen. For the present disclosure, the R1 of the dispersant of Formula I is selected from the alkylphenyl group, the linear or branched group, and the primary or secondary alkyl chain group with a total of 12 to 14 carbon atoms. For the present disclosure, the molar ratio of lithium, iron, and phosphorous within the lithium iron phosphate slurry is approximately 1: 1: 1.
[0028] In some examples, at least one of the R1, R2, and R3 groups of Formula II includes one of a hydroxyl alkyl group having 1-4 carbons. In some examples, at least two of the R1, R2, and R3 groups of Formula II includes one of a hydroxyl alkyl group having 1-4 carbons. In a specific example, the alkanolamine of Formula II is Triisopropanolamine (TIPA) where R1, R2, and R3 groups of Formula II are each an isopropanolamine group. In a specific example, the alkanolamine of Formula II is triethanolamine (TEA) where R1, R2, and R3 groups of Formula II are each an ethanol group. In a specific example, the alkanolamine of Formula II is diethanolamine where R1 is a hydrogen and R2 and R3 groups are ethanol groups. Furthermore, in a specific example, the alkanolamine of Formula II is ethanolamine (MEA) where R1 and R2 groups are hydrogen and R3 group is an ethanol group.
[0029] In some examples, a solid content of the iron compound and the lithium compound is greater than 40 weight percent (wt. %) of the lithium iron phosphate slurry based on the total weight of the lithium iron phosphate slurry, and the lithium iron phosphate slurry has a viscosity of about 150 to about 600 centipoise (cP) , where the viscosity is measured as described in the Examples section herein. For the present disclosure, a solid content of the iron compound and the lithium compound is greater than 50 weight percent (wt. %) of the lithium iron phosphate slurry based on the total weight of the lithium iron phosphate slurry, and the lithium iron phosphate slurry has a viscosity of about 200 to about 700 centipoise (cP) , where the viscosity is measured as described in the Examples section herein.
[0030] For the present disclosure, the iron compound is iron phosphate (FePO4) and the lithium compound is lithium carbonate (Li2CO3) . For the present disclosure, the lithium iron phosphate slurry includes glucose as a carbon source. For the present disclosure, the dispersant of Formula I and the alkanolamine of Formula II are combined with the iron compound, the lithium compound and water to form an aqueous mixture. As described herein, the iron compound and the lithium compound can be the active materials within the aqueous mixture. In this way, the iron compound and lithium compound can be 50 wt. %of the aqueous mixture.
[0031] In some examples, the dispersant comprises 0.5 weight percent to about 5.0 weight percent of a total weight of both the active materials (e.g., combined weight of iron compound and lithium compound, etc. ) . For the present disclosure, the dispersant comprises 0.8 weight percent to 4.0 weight percent of a total weight of both the iron compound and the lithium compound. For the present disclosure, the alkanolamine is present in the slurry from 10 molar percent to 120 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In some examples, the alkanolamine is present in the slurry from 10 molar percent to 25 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In other examples, the alkanolamine is present in the slurry from 25 molar percent to 50 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In further examples, the alkanolamine is present in the slurry from 75 molar percent to 100 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In further examples, the alkanolamine is present in the slurry from 100 molar percent to 120 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I.
[0032] The present disclosure further includes a method that includes generating a lithium iron phosphate slurry including: combining an iron compound and a lithium compound, water, a carbon source with a weight percent that is greater than 40 weight percent of the lithium iron phosphate slurry, combining a dispersant of Formula I:
[0033] where n of Formula I is an integer from 1 to 10 and R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C1 to C18 alkyl chain and R2 of Formula I is selected from a group consisting of a hydrogen, a methyl group, an ethyl group or combinations thereof, and combining an alkanolamine of Formula II:
[0034] where R1, R2, and R3 of Formula II is independently selected from a hydrogen or a hydroxyl alkyl group having 1 to 4 carbons.
[0035] In some examples, the n of Formula I is an integer from 3 to 8. In other examples, the n of Formula I is one of 5 or 7.5. In some examples, R1 of Formula I is a C10 to C16 alkylphenyl group. In a specific example, the R1 of Formula I is a C14 alkylphenyl group. In a specific example, the R2 group of Formula I is a hydrogen. For the present disclosure, the R1 of the dispersant of Formula I is selected from the alkylphenyl group, the linear or branched group, and the primary or secondary alkyl chain group with a total of 12 to 14 carbon atoms. For the present disclosure, the molar ratio of lithium, iron, and phosphorous within the lithium iron phosphate slurry is approximately 1: 1: 1.
[0036] In some examples, at least one of the R1, R2, and R3 groups of Formula II includes one of a hydroxyl alkyl group having 1-4 carbons. In some examples, at least two of the R1, R2, and R3 groups of Formula II includes one of a hydroxyl alkyl group having 1-4 carbons. In a specific example, the alkanolamine of Formula II is Triisopropanolamine (TIPA) where R1, R2, and R3 groups of Formula II are each an isopropanolamine group. In a specific example, the alkanolamine of Formula II is triethanolamine (TEA) where R1, R2, and R3 groups of Formula II are each an ethanol group. In a specific example, the alkanolamine of Formula II is diethanolamine where R1 is a hydrogen and R2 and R3 groups are ethanol groups. Furthermore, in a specific example, the alkanolamine of Formula II is ethanolamine (MEA) where R1 and R2 groups are hydrogen and R3 group is an ethanol group.
[0037] The method further includes performing a spray-drying process on the lithium iron phosphate slurry when a viscosity of the lithium iron phosphate slurry is less than 400 centipoise (cP) and calcinating the lithium iron phosphate mixture, where the viscosity is measured as described in the Examples section herein. For the present disclosure, the iron compound is iron phosphate (FePO4) and the lithium compound is lithium carbonate (Li2CO3) . For the present disclosure, the composition of dispersant of Formula I is within a range of 0.8 weight percent to 4.0 weight percent with respective to a total amount of active materials including the iron phosphate (FePO4) and the lithium carbonate (Li2CO3) and the composition of the alkanolamine of Formula II is within a range of 10 molar percent to 120 molar percent with respect to a molar quantity of P (OH) sites in the dispersant of Formula I. In some examples, the alkanolamine is present in the slurry from 10 molar percent to 25 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In other examples, the alkanolamine is present in the slurry from 25 molar percent to 50 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In further examples, the alkanolamine is present in the slurry from 75 molar percent to 100 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I. In further examples, the alkanolamine is present in the slurry from 100 molar percent to 120 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I.
[0038] For the present disclosure, the weight percent of the iron phosphate (FePO4) and the lithium carbonate (Li2CO3) is greater than 45 weight percent of the lithium iron phosphate slurry and the viscosity of the lithium iron phosphate slurry is less than 200 cP, where the viscosity is measured as described in the Examples section herein. For the present disclosure, the carbon source is glucose. For the present disclosure, R1 of the dispersant of Formula I is one of an octyl phenyl or nonyl phenyl.
[0039] Examples
[0040] In the Examples, various terms and designations for materials were used including, for example, the following:
[0041] Materials
[0042] Materials employed in the examples (EX) and / or comparative examples (CE) include the following.
[0043] Table 1. Ingredients of this disclosure
[0044] Table 2. Chemical Structures of this disclosure
[0045] Table 3. Formulations of this disclosure
[0046] Table 3. Continued
[0047] Preparation of Lithium Iron Phosphate (LFP) Slurry
[0048] The composition of the phosphoric acid ester dispersant can range from 0.8 to 4.0 weight percent (wt. %) with respect to the total amount of active materials added (FePO4 + Li2CO3) . The composition of amine can range from 10 to 120 molar %with respect to the amount of P (OH) sites in phosphoric acid ester dispersant.
[0049] The formulations are as shown in Table 3. The total active material solid content is set to be 50 wt. %, and water is used as the solvent. FePO4 is used as the Fe source and P source, while Li2CO3 is used as the Li source. The molar ratio of Li: Fe: P is about 1: 1: 1. Glucose is used as the carbon source in these examples to increase electronic conductivity of LFP slurry produced.
[0050] The procedure of preparing LFP precursor slurry (e.g., LFP mixture, LFP precursor mixture) is as follows. FePO4 and Li2CO3 were first pre-dispersed in water at 1000 rpm for 2 min using Speedmixer DAC 150. Glucose was then added to the mixture and mixed until completely dissolved. The remaining ingredients as indicated in each formulation were added into the mixture and mixed until completely dissolved. The mixture was transferred to a milling cylinder to perform a sand milling process. Sand milling is the process of adding milling beads to the solid materials and mixing them together at a relatively high speed. The laboratory-scale sand mill for the sand milling process utilizes 1400 rotations per minute (rpm) . The cylinder is 200 milliliters (mL) and is surrounded by flowing cooling water during the milling process. A 1: 1 mass ratio of zirconia bead (with a diameter of 0.8~1.2 mm) was added to the milling cylinder. The mixture was sand milled for 8 hours at room temperature (approximately 22 Celsius) . If foaming was observed during the process, additional defoamer was added. After sand-milling, all beads were filtered out and the viscosity of the LFP precursor slurry was measured using a Brookfield Viscometer DV-II+ Pro at room temperature (approximately 22 Celsius) . The rotation speed was set as 60 1 / sduring measurement. The cap used was Cone Spindle #10.
[0051] Data Analysis
[0052] CE1 represents a formulation with no dispersants or amine (alkanolamine) added. The viscosity of the LFP precursor was measured at 802 centipoise (cP) after sand milling for 8 hr. CE1 is used as a baseline for future comparison study regarding the effect of viscosity reduction in LFP precursor slurry. CE2 represents the formulation with only phosphoric acid ester added and no amine. Comparing CE2 with CE1, the viscosity of the LFP precursor slurry of CE2 is even higher than the baseline example of CE1. IE1, IE2, IE3 and IE4 are inventive examples using Dispersant 1 as the phosphoric acid ester and Ethanolamine (MEA) as the alkanolamine, with varying molar ratio of amine to P (OH) sites (120%, 100%, 75%and 50%respectively) . When comparing with CE1, the IE1, IE2, IE3 and IE4 examples are effective in reducing LFP precursor slurry viscosity. For example, CE1 had a measured viscosity of 802 cP while IE1 had a measured viscosity of 640 cP, IE2 had a measured viscosity of 406 cP, IE3 had a measured viscosity of 632 cP, and IE4 had a measured viscosity of 426 cP. IE5 is an inventive example also using Dispersant 1 as the phosphoric acid ester and 25 mol%DEA as the alkanolamine. When comparing with examples CE1 and CE2, the IE5 example is effective in reducing LFP precursor slurry viscosity. For example, CE1 had a measured viscosity of 802 cP and CE2 had a measured viscosity of 1096 cP, while the IE5 example had a measured viscosity of 704 cP. IE6 and IE7 are the inventive examples using Dispersant 1 as the phosphoric acid ester and Triethanolamine (TEA) as the alkanolamine, with 16.5%and 10%molar ratio of amine to P (OH) sites respectively. When compared with CE1 and CE2, it is observed that both IE6 and IE7 are effective in reducing LFP precursor slurry viscosity. For example, CE1 had a measured viscosity of 802 cP and CE2 had a measured viscosity of 1096 cP, while the IE6 example had a measured viscosity of 153 cP and the IE7 example had a measured viscosity of 356 cP. IE8 is another inventive example using Dispersant 1 as the phosphoric acid ester and 25 mol%Triisopropanolamine (TIPA) as the alkanolamine. When comparing with examples CE1 and CE2, the IE8 example is effective in reducing LFP precursor slurry viscosity. For example, CE1 had a measured viscosity of 802 cP and CE2 had a measured viscosity of 1096 cP, while the IE8 example had a measured viscosity of 226 cP. IE9 and IE10 are inventive examples varying the ratio of phosphoric acid ester Dispersant 1. When the composition of phosphoric acid ester Dispersant 1 changes from 3.2 wt. %to 0.8 wt. % (with respect to the amount of active material (FePO4 + Li2CO3) ) , the IE9 and IE10 examples are still effective in reducing LFP viscosity compared with that of CE1. For example, CE1 had a measured viscosity of 802 cP, while the IE9 example had a measured viscosity of 668 cP and the IE10 example had a measured viscosity of 594 cP. IE11 and IE12 are inventive examples varying the type of phosphoric acid ester used. In these cases, Dispersant 2 is used at 3.2 wt. %ratio with varying types of amines. When comparing with examples CE1 and CE2, the IE11 and IE12 examples are effective in reducing LFP precursor slurry viscosity. For example, CE1 had a measured viscosity of 802 cP and CE2 had a measured viscosity of 1096 cP, while the IE11 example had a measured viscosity of 612 cP and the IE12 example had a measured viscosity of 532 cP.
Claims
1.A lithium iron phosphate slurry, comprising:an iron compound;a lithium compound;a dispersant of Formula I:wherein n of Formula I is an integer from 1 to 10 and R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C1 to C18 alkyl chain and R2 of Formula I is selected from a group consisting of a hydrogen, a methyl group, an ethyl group or combinations thereof; andan alkanolamine of Formula II:wherein R1, R2, and R3 of Formula II is independently selected from a hydrogen or a hydroxyl alkyl group having 1 to 4 carbons.2.The lithium iron phosphate slurry of claim 1, wherein a solid content of the iron compound and the lithium compound is greater than 50 weight percent (wt. %) of the lithium iron phosphate slurry based on the total weight of the lithium iron phosphate slurry, and the lithium iron phosphate slurry has a viscosity of about 200 to about 700 centipoise (cP) .3.The lithium iron phosphate slurry of any one of claims 1-2, wherein the iron compound is iron phosphate (FePO4) and the lithium compound is lithium carbonate (Li2CO3) .4.The lithium iron phosphate slurry of any one of claims 1-3, wherein the lithium iron phosphate slurry includes glucose as a carbon source.5.The lithium iron phosphate slurry of any one of claims 1-4, wherein the dispersant of Formula I and the alkanolamine of Formula II are combined with the iron compound, the lithium compound and water to form an aqueous mixture.6.The lithium iron phosphate slurry of any one of claims 1-5, wherein the dispersant comprises 0.8 weight percent to 4.0 weight percent of a total weight of both the iron compound and the lithium compound.7.The lithium iron phosphate slurry of any one of claims 1-6, wherein the alkanolamine is present in the slurry from 10 molar percent to 120 molar percent of a molar quantity of P (OH) sites of the dispersant of Formula I.8.The lithium iron phosphate slurry of any one of claims 1-6, wherein the R1 of the dispersant of Formula I is selected from the alkylphenyl group, the linear or branched group, and the primary or secondary alkyl chain group with a total of 12 to 14 carbon atoms.9.The lithium iron phosphate slurry of any one of claims 1-8, wherein the molar ratio of lithium, iron, and phosphorous within the lithium iron phosphate slurry is approximately 1∶ 1∶ 1.10.A method, comprising:generating a lithium iron phosphate slurry including:combining an iron compound and a lithium compound, water, a carbon source with a weight percent that is greater than 40 weight percent of the lithium iron phosphate slurry;combining a dispersant of Formula I:wherein n of Formula I is an integer from 1 to 10 and R1 of Formula I is selected from a group consisting of a hydrogen, a C8 to C18 alkylphenyl group, a linear or branched primary or secondary C1 to C18 alkyl chain and R2 of Formula I is selected from a group consisting of a hydrogen, a methyl group, an ethyl group or combinations thereof; andcombining an alkanolamine of Formula II:wherein R1, R2, and R3 of Formula II is independently selected from a hydrogen or a hydroxyl alkyl group having 1 to 4 carbons;performing a spray-drying process on the lithium iron phosphate slurry when a viscosity of the lithium iron phosphate slurry is less than 400 centipoise (cP) ; andcalcinating the lithium iron phosphate mixture.11.The method of claim 10, wherein the iron compound is iron phosphate (FePO4) and the lithium compound is lithium carbonate (Li2CO3) .12.The method of any one of claims 10-11, wherein the composition of dispersant of Formula I is within a range of 0.8 weight percent to 4.0 weight percent with respective to a total amount of active materials including the iron phosphate (FePO4) and the lithium carbonate (Li2CO3) and the composition of the alkanolamine of Formula II is within a range of 10 molar percent to 120 molar percent with respect to a molar quantity of P (OH) sites in the dispersant of Formula I.13.The method of any one of claims 10-12, wherein the weight percent of the iron phosphate (FePO4) and the lithium carbonate (Li2CO3) is greater than 45 weight percent of the lithium iron phosphate slurry and the viscosity of the lithium iron phosphate slurry is less than 200 cP.14.The method of any one of claims 10-13, wherein the carbon source is glucose.15.The method of any one of claims 10-14, wherein R1 of the dispersant of Formula I is one of an octyl phenyl or nonyl phenyl.
Citation Information
Patent Citations
All-solid secondary battery binder composition, all-solid secondary battery slurry composition, solid-electrolyte-containing layer, and all-solid secondary battery
EP3859857A1
Cathode slurry composition for secondary battery, cathode manufactured using same, and secondary battery comprising said cathode
EP4195320A1
Lithium solid-state battery
US20210351433A1
Method for preparing carbon-coated lithium iron phosphate material from ferrous phosphate
US20230080632A1